#------------------------------------------------------------------------------ #$Date: 2024-06-01 01:16:21 +0300 (Sat, 01 Jun 2024) $ #$Revision: 292136 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571753.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1571753 loop_ _publ_author_name 'Swain, Asim' 'Radacki, Krzysztof' 'Braunschweig, Holger' 'Ravat, Prince' _publ_section_title ; Helically twisted nanoribbons via stereospecific annulative \p-extension reaction employing [7]helicene as a molecular wrench ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC01814A _journal_year 2024 _chemical_formula_moiety 'C68 H70, 2(C H2 Cl2)' _chemical_formula_sum 'C70 H74 Cl4' _chemical_formula_weight 1057.09 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2022-07-19 _audit_creation_method 'CIF-fill 1.3e (K.Radacki, 2005-22)' _audit_update_record ; 2023-12-18 deposited with the CCDC. 2024-05-29 downloaded from the CCDC. ; _cell_angle_alpha 66.4050(10) _cell_angle_beta 76.5680(10) _cell_angle_gamma 74.1110(10) _cell_formula_units_Z 2 _cell_length_a 14.16160(10) _cell_length_b 14.61250(10) _cell_length_c 15.92860(10) _cell_measurement_reflns_used 74644 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 73.5530 _cell_measurement_theta_min 3.0540 _cell_volume 2876.94(4) _computing_cell_refinement 'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector HPA _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HyPix Arc150' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): -------------------------------------------------------------------------- 1 \w 29.00 54.00 0.50 0.50 -- 58.61 -95.00 -77.00 50 2 \w -56.00 -30.00 0.50 0.50 -- -60.19 95.00 32.00 52 3 \w -76.00 -51.00 0.50 0.50 -- -69.72 95.00 32.00 50 4 \w 30.00 56.00 0.50 0.50 -- 71.30 -95.00 -77.00 52 5 \w -84.00 -58.00 0.50 1.10 -- -76.37 95.00 32.00 52 6 \w 40.00 65.00 0.50 1.10 -- 82.31 -95.00 -77.00 50 7 \w 12.00 37.00 0.50 0.50 -- 2.00 66.00 68.04 50 8 \w 12.00 37.00 0.50 0.50 -- 2.00 66.00 171.80 50 9 \w 16.00 41.00 0.50 0.50 -- 6.00 65.00 -96.15 50 10 \w 16.00 41.00 0.50 0.50 -- 6.00 65.00 -55.45 50 11 \w 16.00 41.00 0.50 0.50 -- 6.00 65.00-162.60 50 12 \w 17.00 42.00 0.50 0.50 -- 6.00 64.00 106.85 50 13 \w 17.00 42.00 0.50 0.50 -- 6.00 64.00 -19.08 50 14 \w 21.00 46.00 0.50 0.50 -- 10.00 62.00 7.10 50 15 \w -44.00 -19.00 0.50 0.50 -- -14.00 130.00 -78.45 50 16 \w 25.00 50.00 0.50 0.50 -- 14.00 61.00-129.22 50 17 \w 25.00 50.00 0.50 0.50 -- 14.00 61.00 133.43 50 18 \w 25.00 50.00 0.50 0.50 -- 14.00 61.00 53.54 50 19 \w -48.00 -23.00 0.50 0.50 -- -18.00 130.00 45.23 50 20 \w 30.00 55.00 0.50 0.50 -- 18.00 60.00 90.24 50 21 \w 30.00 55.00 0.50 0.50 -- 18.00 59.00 -82.54 50 22 \w 30.00 55.00 0.50 0.50 -- 18.00 60.00-164.10 50 23 \w 30.00 55.00 0.50 0.50 -- 18.00 58.00 163.50 50 24 \w 34.00 59.00 0.50 0.50 -- 22.00 58.00 -4.96 50 25 \w 34.00 59.00 0.50 0.50 -- 22.00 58.00 -55.35 50 26 \w 34.00 59.00 0.50 0.50 -- 22.00 58.00 139.61 50 27 \w 34.00 59.00 0.50 0.50 -- 22.00 59.00-101.14 50 28 \w 34.00 59.00 0.50 0.50 -- 22.00 57.00 -28.76 50 29 \w 34.00 59.00 0.50 0.50 -- 22.00 59.00 107.65 50 30 \w 34.00 59.00 0.50 0.50 -- 22.00 57.00 43.73 50 31 \w 34.00 59.00 0.50 0.50 -- 22.00 57.00 66.73 50 32 \w 34.00 59.00 0.50 0.50 -- 22.00 57.00-124.00 50 33 \w 34.00 59.00 0.50 0.50 -- 22.00 59.00 14.55 50 34 \w -64.00 -39.00 0.50 0.50 -- -26.00 -51.00-149.29 50 35 \w 39.00 64.00 0.50 0.50 -- 26.00 52.00-154.61 50 36 \w 39.00 64.00 0.50 0.50 -- 26.00 52.00-100.33 50 37 \w -74.00 -48.00 0.50 0.50 -- -30.00 -47.00 -98.58 52 38 \w -74.00 -48.00 0.50 0.50 -- -34.00 -52.00 4.70 52 39 \w -74.00 -48.00 0.50 0.50 -- -34.00 -51.00-102.28 52 40 \w 47.00 72.00 0.50 0.50 -- 34.00 52.00 175.65 50 41 \w 48.00 73.00 0.50 0.50 -- 34.00 51.00 -37.60 50 42 \w 48.00 73.00 0.50 0.50 -- 34.00 51.00 165.67 50 43 \w 48.00 73.00 0.50 0.50 -- 34.00 51.00-135.25 50 44 \w -79.00 -53.00 0.50 0.50 -- -38.00 -49.00 -52.40 52 45 \w -79.00 -53.00 0.50 0.50 -- -38.00 -50.00 34.10 52 46 \w -81.00 -55.00 0.50 0.50 -- -38.00 -49.00 -27.19 52 47 \w 51.00 76.00 0.50 0.50 -- 38.00 52.00 139.74 50 48 \w 52.00 77.00 0.50 0.50 -- 38.00 50.00 -96.73 50 49 \w 52.00 77.00 0.50 0.50 -- 38.00 50.00-169.36 50 50 \w 51.00 76.00 0.50 0.50 -- 38.00 52.00-109.36 50 51 \w 51.00 76.00 0.50 0.50 -- 38.00 52.00-151.54 50 52 \w 51.00 76.00 0.50 0.50 -- 38.00 52.00 -84.42 50 53 \w 56.00 81.00 0.50 0.50 -- 42.00 51.00-132.73 50 54 \w 55.00 80.00 0.50 0.50 -- 42.00 52.00 29.57 50 55 \w 55.00 80.00 0.50 0.50 -- 42.00 52.00 89.81 50 56 \w 55.00 80.00 0.50 0.50 -- 42.00 52.00 -10.47 50 57 \w -85.00 -59.00 0.50 0.50 -- -46.00 -51.00 63.90 52 58 \w -86.00 -60.00 0.50 0.50 -- -46.00 -52.00 -3.66 52 59 \w 59.00 84.00 0.50 0.50 -- 46.00 52.00 -90.20 50 60 \w 59.00 84.00 0.50 0.50 -- 46.00 52.00 149.03 50 61 \w -89.00 -63.00 0.50 0.50 -- -50.00 -52.00-109.29 52 62 \w -89.00 -63.00 0.50 0.50 -- -50.00 -45.00 158.81 52 63 \w -89.00 -63.00 0.50 0.50 -- -50.00 -52.00 153.37 52 64 \w -94.00 -68.00 0.50 0.50 -- -54.00 -52.00 134.64 52 65 \w -94.00 -68.00 0.50 0.50 -- -54.00 -50.00-169.28 52 66 \w -93.00 -67.00 0.50 0.50 -- -54.00 -52.00 41.76 52 67 \w -92.00 -67.00 0.50 0.50 -- -54.00 -52.00 25.80 50 68 \w -93.00 -67.00 0.50 0.50 -- -54.00 -52.00 -84.55 52 69 \w -94.00 -68.00 0.50 0.50 -- -54.00 -50.00 -32.27 52 70 \w -94.00 -68.00 0.50 0.50 -- -54.00 -52.00 112.95 52 71 \w -95.00 -69.00 0.50 0.50 -- -54.00 -52.00 -68.56 52 72 \w -93.00 -67.00 0.50 0.50 -- -54.00 -52.00 81.92 52 73 \w -94.00 -68.00 0.50 0.50 -- -54.00 -51.00 -40.87 52 74 \w -98.00 -72.00 0.50 0.50 -- -58.00 -51.00 -47.42 52 75 \w -98.00 -72.00 0.50 0.50 -- -58.00 -52.00 129.26 52 76 \w -97.00 -72.00 0.50 0.50 -- -58.00 -49.00 65.05 50 77 \w -97.00 -71.00 0.50 0.50 -- -58.00 -52.00-135.68 52 78 \w -97.00 -71.00 0.50 0.50 -- -58.00 -51.00-130.24 52 79 \w -98.00 -72.00 0.50 0.50 -- -58.00 -47.00 9.34 52 80 \w -99.00 -73.00 0.50 0.50 -- -58.00 -52.00-150.64 52 81 \w -98.00 -72.00 0.50 0.50 -- -58.00 -50.00-118.70 52 82 \w -96.00 -71.00 0.50 0.50 -- -58.00 -52.00-172.71 50 83 \w 23.00 51.00 0.50 0.50 -- 58.61-126.00 -60.00 56 84 \w 16.00 51.00 0.50 0.50 -- 58.61 -95.00 30.00 70 85 \w 20.00 52.00 0.50 0.50 -- 58.61-126.00-180.00 64 86 \w 17.00 45.00 0.50 0.50 -- 58.61 -95.00 -30.00 56 87 \w -39.00 -14.00 0.50 0.50 -- -60.19 126.00 -60.00 50 88 \w -69.00 -22.00 0.50 0.50 -- -60.19 126.00 150.00 94 89 \w -102.00 -76.00 0.50 0.50 -- -62.00 -48.00 -15.94 52 90 \w -103.00 -77.00 0.50 0.50 -- -62.00 -50.00 104.25 52 91 \w -104.00 -78.00 0.50 0.50 -- -62.00 -47.00-106.37 52 92 \w -106.00 -80.00 0.50 0.50 -- -66.00 -48.00 0.13 52 93 \w -109.00 -83.00 0.50 0.50 -- -70.00 -56.00-164.13 52 94 \w -110.00 -84.00 0.50 0.50 -- -70.00 -56.00 -66.09 52 95 \w -110.00 -84.00 0.50 0.50 -- -70.00 -56.00 64.58 52 96 \w -109.00 -83.00 0.50 0.50 -- -70.00 -55.00 75.21 52 97 \w -109.00 -83.00 0.50 0.50 -- -70.00 -56.00 87.21 52 98 \w -112.00 -86.00 0.50 1.10 -- -74.00 -59.00 12.05 52 99 \w -114.00 -86.00 0.50 1.10 -- -74.00 -59.00 46.22 56 100 \w -112.00 -86.00 0.50 1.10 -- -74.00 -58.00 55.93 52 101 \w -112.00 -86.00 0.50 1.10 -- -74.00 -55.00-177.73 52 102 \w -113.00 -87.00 0.50 1.10 -- -74.00 -59.00 -71.46 52 103 \w -114.00 -88.00 0.50 1.10 -- -74.00 -55.00-117.89 52 104 \w -112.00 -86.00 0.50 1.10 -- -74.00 -58.00 -42.20 52 105 \w -112.00 -86.00 0.50 1.10 -- -74.00 -57.00 -78.45 52 106 \w -115.00 -89.00 0.50 1.10 -- -74.00 -59.00 138.49 52 107 \w -115.00 -88.00 0.50 1.10 -- -74.00 -59.00 -94.21 54 108 \w -113.00 -87.00 0.50 1.10 -- -74.00 -60.00 115.17 52 109 \w -112.00 -86.00 0.50 1.10 -- -74.00 -56.00-170.23 52 110 \w -113.00 -87.00 0.50 1.10 -- -74.00 -58.00 -4.19 52 111 \w -114.00 -88.00 0.50 1.10 -- -74.00 -59.00 167.27 52 112 \w -112.00 -86.00 0.50 1.10 -- -74.00 -57.00 27.29 52 113 \w -113.00 -87.00 0.50 1.10 -- -74.00 -53.00-159.32 52 114 \w -116.00 -90.00 0.50 1.10 -- -78.00 -59.00 -23.87 52 115 \w -118.00 -92.00 0.50 1.10 -- -79.50 -63.00 -51.13 52 116 \w -123.00 -91.00 0.50 1.10 -- -79.50 -60.00-113.79 64 117 \w -124.00 -94.00 0.50 1.10 -- -79.50 -64.00 -92.10 60 118 \w -117.00 -91.00 0.50 1.10 -- -79.50 -60.00 -43.49 52 119 \w -119.00 -92.00 0.50 1.10 -- -79.50 -60.00-173.18 54 120 \w -125.00 -91.00 0.50 1.10 -- -79.50 -60.00 -81.22 68 121 \w -117.00 -91.00 0.50 1.10 -- -79.50 -58.00 8.76 52 122 \w -122.00 -91.00 0.50 1.10 -- -79.50 -59.00 177.61 62 123 \w -126.00-100.00 0.50 1.10 -- -79.50-124.00 50.42 52 124 \w -118.00 -91.00 0.50 1.10 -- -79.50 -56.00 17.51 54 125 \w -122.00 -93.00 0.50 1.10 -- -79.50 -60.00 100.15 58 126 \w -125.00 -97.00 0.50 1.10 -- -79.50-134.00 157.43 56 127 \w -120.00 -94.00 0.50 1.10 -- -79.50 -60.00 86.80 52 128 \w -129.00 -93.00 0.50 1.10 -- -79.50 -48.00-138.84 72 129 \w -121.00 -90.00 0.50 1.10 -- -79.50 -62.00 64.47 62 130 \w -123.00 -96.00 0.50 1.10 -- -79.50-129.00 -19.78 54 131 \w -125.00 -92.00 0.50 1.10 -- -79.50-128.00-176.33 66 132 \w -116.00 -91.00 0.50 1.10 -- -79.50 -58.00 149.70 50 133 \w -100.00 -33.00 0.50 1.10 -- -79.50 122.00-173.75 134 134 \w -116.00 -90.00 0.50 1.10 -- -79.50 -62.00-134.50 52 135 \w -60.00 -32.00 0.50 1.10 -- -79.50 131.00 -11.17 56 136 \w -65.00 -32.00 0.50 1.10 -- -79.50 127.00 40.32 66 137 \w -91.00 -66.00 0.50 1.10 -- -79.50 127.00 40.32 50 138 \w -116.00 -91.00 0.50 1.10 -- -79.50 -58.00 124.50 50 139 \w -118.00 -92.00 0.50 1.10 -- -79.50 -57.00 109.50 52 140 \w -122.00 -91.00 0.50 1.10 -- -79.50 -60.00 -77.93 62 141 \w -57.00 -32.00 0.50 1.10 -- -79.50 134.00 -47.59 50 142 \w -126.00 -88.00 0.50 1.10 -- -79.50-136.00 90.05 76 143 \w -118.00 -92.00 0.50 1.10 -- -79.50 -57.00 -54.01 52 144 \w -97.00 -71.00 0.50 1.10 -- -79.50 134.00 -47.59 52 145 \w -117.00 -91.00 0.50 1.10 -- -79.50 -60.00 -40.19 52 146 \w -123.00 -91.00 0.50 1.10 -- -79.50 -60.00 -9.22 64 147 \w -118.00 -92.00 0.50 1.10 -- -79.50 -63.00 -0.27 52 148 \w -121.00 -94.00 0.50 1.10 -- -79.50 -64.00 171.89 54 149 \w -122.00 -96.00 0.50 1.10 -- -79.50 -60.00 125.54 52 150 \w -121.00 -92.00 0.50 1.10 -- -79.50 -61.00-152.21 58 151 \w -73.00 -33.00 0.50 1.10 -- -79.50 130.00 97.53 80 152 \w -102.00 -33.00 0.50 1.10 -- -79.50 126.00 81.43 138 153 \w -101.00 -33.00 0.50 1.10 -- -79.50 131.00 -76.70 136 154 \w -123.00 -91.00 0.50 1.10 -- -79.50 -59.00 73.79 64 155 \w -117.00 -91.00 0.50 1.10 -- -79.50 -59.00 104.20 52 156 \w -116.00 -90.00 0.50 1.10 -- -79.50 -62.00 38.99 52 157 \w -115.00 -90.00 0.50 1.10 -- -79.50 -62.00 6.37 50 158 \w -115.00 -90.00 0.50 1.10 -- -79.50 -62.00-127.25 50 159 \w -128.00-103.00 0.50 1.10 -- -79.50-118.00 16.46 50 160 \w -118.00 -92.00 0.50 1.10 -- -79.50 -57.00 -29.65 52 161 \w -117.00 -91.00 0.50 1.10 -- -79.50 -59.00 44.23 52 162 \w 40.00 90.00 0.50 1.10 -- 82.31 -95.00 -30.00 100 163 \w 38.00 97.00 0.50 1.10 -- 82.31-112.00 90.00 118 164 \w 46.00 128.00 0.50 1.10 -- 82.31 15.00-120.00 164 165 \w 40.00 97.00 0.50 1.10 -- 82.31-112.00 -90.00 114 166 \w 37.00 97.00 0.50 1.10 -- 82.31-112.00 150.00 120 167 \w 36.00 97.00 0.50 1.10 -- 82.31-112.00 30.00 122 168 \w 69.00 97.00 0.50 1.10 -- 82.31-112.00 120.00 56 169 \w 102.00 127.00 0.50 1.10 -- 82.31 15.00 150.00 50 170 \w 54.00 131.00 0.50 1.10 -- 82.31 15.00 0.00 154 171 \w 72.00 97.00 0.50 1.10 -- 82.31-112.00 0.00 50 172 \w 39.00 97.00 0.50 1.10 -- 82.31-112.00 -30.00 116 173 \w 35.00 96.00 0.50 1.10 -- 82.31-112.00 60.00 122 174 \w 72.00 97.00 0.50 1.10 -- 82.31-112.00 -60.00 50 175 \w 37.00 67.00 0.50 1.10 -- 82.31-112.00 -60.00 60 176 \w 37.00 68.00 0.50 1.10 -- 82.31-112.00 0.00 62 177 \w 41.00 96.00 0.50 1.10 -- 82.31-112.00-180.00 110 178 \w 35.00 97.00 0.50 1.10 -- 82.31-112.00-120.00 124 179 \w 100.00 131.00 0.50 1.10 -- 82.31 15.00 90.00 62 180 \w 46.00 84.00 0.50 1.10 -- 82.31 15.00 90.00 76 181 \w 40.00 101.00 0.50 1.10 -- 85.25-131.00-125.96 122 182 \w 40.00 100.00 0.50 1.10 -- 85.25-133.00 130.81 120 183 \w 99.00 127.00 0.50 1.10 -- 85.25 121.00-163.15 56 184 \w 104.00 132.00 0.50 1.10 -- 85.25 113.00 38.51 56 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-R' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type ; CrysAlisPro convention (1999,Acta A55,543-557) ; _diffrn_orient_matrix_UB_11 -0.0440209000 _diffrn_orient_matrix_UB_12 0.0519031000 _diffrn_orient_matrix_UB_13 -0.0916669000 _diffrn_orient_matrix_UB_21 -0.0731120000 _diffrn_orient_matrix_UB_22 -0.0729811000 _diffrn_orient_matrix_UB_23 0.0375376000 _diffrn_orient_matrix_UB_31 -0.0759111000 _diffrn_orient_matrix_UB_32 0.0760472000 _diffrn_orient_matrix_UB_33 0.0393310000 _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_xray_symbol K-L~2,3~ _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_unetI/netI 0.0098 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.964 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 123212 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.964 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.002 _diffrn_reflns_theta_min 3.057 _diffrn_source 'rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet-R X-ray Source' _exptl_absorpt_coefficient_mu 2.176 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_density_diffrn 1.220 _exptl_crystal_description plate _exptl_crystal_F_000 1124 _exptl_crystal_preparation ; Crystalls were grown from saturated solution of dichloromethane at 23 \%C. For data collection the crystal was immersed in a film of perfluoropolyether oil, mounted on a polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800). ; _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.170 _refine_diff_density_min -1.228 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 687 _refine_ls_number_reflns 11428 _refine_ls_number_restraints 413 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0643 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+3.2811P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1687 _refine_ls_wR_factor_ref 0.1710 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10627 _reflns_number_total 11428 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01814a3.cif _cod_data_source_block KR1112_AsSw_a _cod_database_code 1571753 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.722 _shelx_estimated_absorpt_t_max 0.881 _shelx_res_file ; TITL KR1112_AsSw_a.res in P-1 KR1112_AsSw_a.res created by SHELXL-2018/3 at 11:20:42 on 19-Jul-2022 REM Old TITL KR1112_AsSw in P-1 REM SHELXT solution in P-1 REM R1 0.174, Rweak 0.009, Alpha 0.045, Orientation as input REM Formula found by SHELXT: C70 Cl4 CELL 1.54184 14.1616 14.6125 15.9286 66.405 76.568 74.111 ZERR 2.000 0.0001 0.0001 0.0001 0.001 0.001 0.001 LATT 1 SFAC C H CL UNIT 140.00 148.00 8.00 TEMP -173 SIZE 0.06 0.10 0.16 L.S. 10 BOND $H CONF LIST 4 FMAP 2 PLAN 20 ACTA WGHT 0.080500 3.281100 FVAR 0.30991 0.54157 0.13630 RESI 1 MAIN C1 1 0.295745 0.350739 0.688524 11.00000 0.02799 0.02401 = 0.02232 -0.00340 -0.00475 -0.00481 C2 1 0.239402 0.319735 0.648097 11.00000 0.02894 0.02530 = 0.02005 -0.00174 -0.00778 -0.00313 AFIX 43 H2 2 0.205549 0.368890 0.598527 11.00000 -1.20000 AFIX 0 C3 1 0.231299 0.217419 0.678781 11.00000 0.02300 0.02650 = 0.01982 -0.00726 -0.00278 -0.00272 C4 1 0.172554 0.184695 0.638145 11.00000 0.02566 0.02980 = 0.02257 -0.00566 -0.00745 -0.00272 AFIX 43 H4 2 0.138987 0.233163 0.588113 11.00000 -1.20000 AFIX 0 C5 1 0.164010 0.086073 0.669706 11.00000 0.02446 0.03387 = 0.02518 -0.01060 -0.00703 -0.00531 AFIX 43 H5 2 0.122848 0.067255 0.642558 11.00000 -1.20000 AFIX 0 C6 1 0.215546 0.009246 0.743120 11.00000 0.02252 0.02620 = 0.02328 -0.01030 -0.00425 -0.00121 C7 1 0.203433 -0.092224 0.780445 11.00000 0.02650 0.02823 = 0.03017 -0.01489 -0.00714 -0.00333 AFIX 43 H7 2 0.161111 -0.111799 0.755112 11.00000 -1.20000 AFIX 0 C8 1 0.251469 -0.164553 0.853160 11.00000 0.02857 0.02296 = 0.02878 -0.01287 -0.00570 -0.00143 C9 1 0.320645 -0.135972 0.884030 11.00000 0.02515 0.02142 = 0.02448 -0.00990 -0.00658 0.00080 AFIX 43 H9 2 0.357282 -0.186145 0.931168 11.00000 -1.20000 AFIX 0 C10 1 0.337278 -0.036528 0.847813 11.00000 0.02156 0.02243 = 0.02127 -0.01030 -0.00244 -0.00012 C11 1 0.401341 -0.003999 0.885792 11.00000 0.02154 0.02143 = 0.01913 -0.00745 -0.00262 -0.00170 C12 1 0.482037 -0.075553 0.935622 11.00000 0.02058 0.01899 = 0.01837 -0.00487 -0.00160 -0.00280 C13 1 0.533317 -0.163396 0.916422 11.00000 0.02405 0.02094 = 0.01963 -0.00733 -0.00369 -0.00265 AFIX 43 H13 2 0.511639 -0.179998 0.873099 11.00000 -1.20000 AFIX 0 C14 1 0.615446 -0.227124 0.959343 11.00000 0.02224 0.01769 = 0.02089 -0.00598 -0.00127 -0.00302 C15 1 0.638034 -0.209243 1.031346 11.00000 0.01982 0.01785 = 0.01971 -0.00319 -0.00288 -0.00305 AFIX 43 H15 2 0.688128 -0.256914 1.066411 11.00000 -1.20000 AFIX 0 C16 1 0.588626 -0.122479 1.053484 11.00000 0.01879 0.01868 = 0.01835 -0.00452 -0.00157 -0.00406 C17 1 0.518058 -0.049441 0.996969 11.00000 0.01845 0.01860 = 0.01805 -0.00461 -0.00085 -0.00292 C18 1 0.382048 0.097721 0.877403 11.00000 0.01900 0.02049 = 0.01937 -0.00580 -0.00203 -0.00234 C19 1 0.332234 0.175366 0.800233 11.00000 0.01926 0.02191 = 0.01959 -0.00668 -0.00199 -0.00141 C20 1 0.340670 0.277538 0.765102 11.00000 0.02388 0.02274 = 0.02169 -0.00565 -0.00515 -0.00329 AFIX 43 H20 2 0.378195 0.298365 0.794055 11.00000 -1.20000 AFIX 0 C21 1 0.281766 0.143631 0.752708 11.00000 0.02009 0.02351 = 0.01955 -0.00721 -0.00167 -0.00172 C22 1 0.278317 0.038860 0.781105 11.00000 0.02077 0.02372 = 0.01997 -0.00894 -0.00231 -0.00137 C23 1 0.312045 0.460413 0.652048 11.00000 0.04318 0.02531 = 0.03029 0.00087 -0.01313 -0.01087 C24 1 0.249908 0.531707 0.574949 11.00000 0.09525 0.03171 = 0.05650 0.01174 -0.04686 -0.02328 AFIX 137 H24A 2 0.256622 0.602041 0.558512 11.00000 -1.50000 H24B 2 0.180129 0.526876 0.596443 11.00000 -1.50000 H24C 2 0.273199 0.511842 0.520537 11.00000 -1.50000 AFIX 0 C25 1 0.422097 0.459955 0.616406 11.00000 0.05842 0.04658 = 0.03559 -0.00868 0.00226 -0.02807 AFIX 137 H25A 2 0.433413 0.529607 0.593824 11.00000 -1.50000 H25B 2 0.442197 0.433643 0.565793 11.00000 -1.50000 H25C 2 0.461223 0.416321 0.666756 11.00000 -1.50000 AFIX 0 C26 1 0.281329 0.503263 0.730541 11.00000 0.04539 0.02578 = 0.04624 -0.00802 -0.01251 -0.00457 AFIX 137 H26A 2 0.291692 0.573383 0.706618 11.00000 -1.50000 H26B 2 0.321603 0.460999 0.780310 11.00000 -1.50000 H26C 2 0.211136 0.502687 0.754669 11.00000 -1.50000 AFIX 6 RIGU 0.003 C27_2 > C30_20 SIMU 0.010 C27_2 > C30_20 isor 0.015 C27_2 > C30_20 EADP C28_2 C28_20 EADP C29_2 C29_20 EADP C30_2 C30_20 EADP C27_2 C27_20 SADI 0.002 C8_1 C27_2 C8_1 C27_20 SADI_1 0.003 C8 C28_2 C8 C29_2 C8 C30_2 = C8 C28_20 C8 C29_20 C8 C30_20 part 1 31 RESI 2 TBU C27 1 0.229869 -0.273247 0.904831 31.00000 0.03681 0.02274 = 0.03950 -0.01322 -0.01009 -0.00449 C28 1 0.289676 -0.328811 0.986021 31.00000 0.13655 0.04110 = 0.10294 0.00551 -0.07750 -0.04219 AFIX 137 H28A 2 0.257838 -0.383461 1.032745 31.00000 -1.50000 H28B 2 0.292366 -0.280469 1.013430 31.00000 -1.50000 H28C 2 0.357133 -0.358092 0.963892 31.00000 -1.50000 AFIX 5 C29 1 0.119201 -0.266348 0.941252 31.00000 0.05594 0.02190 = 0.11606 -0.00786 0.02478 -0.00345 AFIX 137 H29A 2 0.094216 -0.313144 0.925834 31.00000 -1.50000 H29B 2 0.083283 -0.196430 0.912688 31.00000 -1.50000 H29C 2 0.109219 -0.285051 1.008564 31.00000 -1.50000 AFIX 5 C30 1 0.259689 -0.332081 0.838837 31.00000 0.09062 0.05477 = 0.05807 -0.02970 0.02925 -0.04747 AFIX 137 H30A 2 0.235788 -0.396193 0.868401 31.00000 -1.50000 H30B 2 0.332073 -0.346867 0.823989 31.00000 -1.50000 H30C 2 0.230307 -0.290868 0.781851 31.00000 -1.50000 AFIX 5 part 2 -31 RESI 20 TBU C27 1 0.229869 -0.273247 0.904831 -31.00000 0.03681 0.02274 = 0.03950 -0.01322 -0.01009 -0.00449 C28 1 0.156036 -0.289349 0.858052 -31.00000 0.13655 0.04110 = 0.10294 0.00551 -0.07750 -0.04219 AFIX 137 H28A 2 0.138571 -0.356151 0.893892 -31.00000 -1.50000 H28B 2 0.186136 -0.286438 0.795306 -31.00000 -1.50000 H28C 2 0.096109 -0.235773 0.854996 -31.00000 -1.50000 AFIX 5 C29 1 0.326511 -0.351814 0.902821 -31.00000 0.05594 0.02190 = 0.11606 -0.00786 0.02478 -0.00345 AFIX 137 H29A 2 0.312364 -0.420633 0.932133 -31.00000 -1.50000 H29B 2 0.372125 -0.344566 0.936509 -31.00000 -1.50000 H29C 2 0.356947 -0.340565 0.838533 -31.00000 -1.50000 AFIX 5 C30 1 0.186020 -0.286079 1.005236 -31.00000 0.09062 0.05477 = 0.05807 -0.02970 0.02925 -0.04747 AFIX 137 H30A 2 0.174389 -0.355583 1.038778 -31.00000 -1.50000 H30B 2 0.123115 -0.237114 1.006582 -31.00000 -1.50000 H30C 2 0.232470 -0.273759 1.034660 -31.00000 -1.50000 AFIX 0 resi 0 part 0 C31 1 0.679611 -0.311152 0.923680 11.00000 0.02558 0.02109 = 0.02425 -0.00964 -0.00316 0.00113 C32 1 0.614915 -0.375884 0.916808 11.00000 0.03410 0.02838 = 0.04030 -0.02028 -0.01124 0.00224 AFIX 137 H32A 2 0.657128 -0.429713 0.895068 11.00000 -1.50000 H32B 2 0.567913 -0.332510 0.873106 11.00000 -1.50000 H32C 2 0.578346 -0.406809 0.977856 11.00000 -1.50000 AFIX 0 C33 1 0.758470 -0.381342 0.985340 11.00000 0.03263 0.02511 = 0.04043 -0.01740 -0.01282 0.00615 AFIX 137 H33A 2 0.795543 -0.435199 0.961454 11.00000 -1.50000 H33B 2 0.726327 -0.412150 1.048566 11.00000 -1.50000 H33C 2 0.804062 -0.341647 0.985504 11.00000 -1.50000 AFIX 0 C34 1 0.732639 -0.259751 0.826579 11.00000 0.04189 0.03234 = 0.03183 -0.01162 0.00869 0.00180 AFIX 137 H34A 2 0.772896 -0.312090 0.802005 11.00000 -1.50000 H34B 2 0.775539 -0.219326 0.830125 11.00000 -1.50000 H34C 2 0.683311 -0.215045 0.785658 11.00000 -1.50000 AFIX 0 RESI 0 RESI 11 MAIN C1 1 0.408613 0.318611 0.353949 11.00000 0.02741 0.02170 = 0.02475 -0.01124 -0.00446 0.00064 C2 1 0.459595 0.389209 0.284791 11.00000 0.02194 0.02701 = 0.02811 -0.01296 -0.00226 0.00069 AFIX 43 H2 2 0.526277 0.366742 0.261461 11.00000 -1.20000 AFIX 0 C3 1 0.415325 0.492777 0.248447 11.00000 0.02254 0.02452 = 0.02289 -0.01011 -0.00323 -0.00369 C4 1 0.467256 0.566850 0.177082 11.00000 0.02198 0.03006 = 0.02643 -0.01058 -0.00006 -0.00476 AFIX 43 H4 2 0.532934 0.544935 0.151158 11.00000 -1.20000 AFIX 0 C5 1 0.424429 0.667399 0.145982 11.00000 0.02489 0.02668 = 0.02391 -0.00700 0.00031 -0.00862 AFIX 43 H5 2 0.459686 0.714188 0.097151 11.00000 -1.20000 AFIX 0 C6 1 0.326663 0.704322 0.185640 11.00000 0.02457 0.02254 = 0.02104 -0.00822 -0.00223 -0.00652 C7 1 0.282131 0.808461 0.155630 11.00000 0.02813 0.02188 = 0.02022 -0.00538 -0.00077 -0.00915 AFIX 43 H7 2 0.317622 0.856012 0.108049 11.00000 -1.20000 AFIX 0 C8 1 0.187481 0.843368 0.193953 11.00000 0.02922 0.01849 = 0.02098 -0.00625 -0.00369 -0.00580 C9 1 0.139018 0.772421 0.268217 11.00000 0.02504 0.01846 = 0.02029 -0.00735 -0.00203 -0.00451 AFIX 43 H9 2 0.074816 0.795958 0.295830 11.00000 -1.20000 AFIX 0 C10 1 0.181639 0.668486 0.303064 11.00000 0.02335 0.01836 = 0.01960 -0.00753 -0.00316 -0.00517 C11 1 0.130683 0.593198 0.378209 11.00000 0.02176 0.01662 = 0.01909 -0.00636 -0.00375 -0.00326 C12 1 0.053067 0.619132 0.447998 11.00000 0.02138 0.01497 = 0.01809 -0.00465 -0.00440 -0.00188 C13 1 0.046971 0.703695 0.471882 11.00000 0.02304 0.01393 = 0.02004 -0.00478 -0.00366 -0.00301 AFIX 43 H13 2 0.089702 0.750083 0.436737 11.00000 -1.20000 AFIX 0 C14 1 -0.020222 0.721053 0.545837 11.00000 0.02503 0.01347 = 0.02087 -0.00620 -0.00580 -0.00150 C15 1 -0.091427 0.660428 0.588865 11.00000 0.02382 0.01552 = 0.01863 -0.00604 -0.00255 -0.00138 AFIX 43 H15 2 -0.142831 0.677089 0.633829 11.00000 -1.20000 AFIX 0 C16 1 -0.088833 0.575619 0.567279 11.00000 0.02282 0.01444 = 0.01785 -0.00458 -0.00454 -0.00167 C17 1 -0.008573 0.548706 0.504130 11.00000 0.02184 0.01442 = 0.01784 -0.00517 -0.00469 -0.00214 C18 1 0.159068 0.491649 0.384638 11.00000 0.02350 0.01687 = 0.01744 -0.00630 -0.00295 -0.00291 C19 1 0.260128 0.454608 0.347558 11.00000 0.02328 0.01859 = 0.01942 -0.00903 -0.00342 -0.00271 C20 1 0.308321 0.351904 0.382087 11.00000 0.02599 0.01802 = 0.02213 -0.00829 -0.00205 -0.00297 AFIX 43 H20 2 0.271459 0.303333 0.426127 11.00000 -1.20000 AFIX 0 C21 1 0.316690 0.526767 0.284273 11.00000 0.02289 0.01982 = 0.01987 -0.00866 -0.00386 -0.00328 C22 1 0.274391 0.633287 0.256959 11.00000 0.02338 0.01990 = 0.02006 -0.00817 -0.00343 -0.00533 RIGU 0.003 C23_12 > C26_120 SIMU 0.010 C23_12 > C26_120 isor 0.015 C23_12 > C26_120 EADP C24_12 C24_120 EADP C25_12 C25_120 EADP C26_12 C26_120 EADP C23_12 C23_120 REM Exyz C23_12 C23_120 sadi 0.002 C1_11 C23_12 C1_11 C23_120 PART 1 21 ! #################### resi 12 tbu AFIX 6 C23 1 0.459734 0.207246 0.404838 21.00000 0.03131 0.02215 = 0.02987 -0.00944 -0.00713 0.00448 C24 1 0.563417 0.180789 0.354384 21.00000 0.05404 0.03529 = 0.06069 0.00887 0.01628 0.02126 AFIX 137 H24A 2 0.585943 0.106534 0.375499 21.00000 -1.50000 H24B 2 0.609423 0.210939 0.367737 21.00000 -1.50000 H24C 2 0.561294 0.207948 0.287599 21.00000 -1.50000 AFIX 5 C25 1 0.467756 0.196641 0.502590 21.00000 0.06148 0.03102 = 0.03924 -0.01250 -0.01597 0.01296 AFIX 137 H25A 2 0.503543 0.127834 0.534879 21.00000 -1.50000 H25B 2 0.401138 0.208357 0.536537 21.00000 -1.50000 H25C 2 0.503726 0.246938 0.498969 21.00000 -1.50000 AFIX 5 C26 1 0.396664 0.134523 0.410489 21.00000 0.08068 0.02750 = 0.09042 -0.01412 -0.05568 0.00539 AFIX 137 H26A 2 0.425698 0.064634 0.447513 21.00000 -1.50000 H26B 2 0.394762 0.138375 0.348033 21.00000 -1.50000 H26C 2 0.329134 0.153979 0.439542 21.00000 -1.50000 AFIX 6 PART 2 -21 ! #################### resi 120 tbu C23 1 0.462984 0.207153 0.398899 -21.00000 0.03131 0.02215 = 0.02987 -0.00944 -0.00713 0.00448 C24 1 0.392179 0.140204 0.468297 -21.00000 0.05404 0.03529 = 0.06069 0.00887 0.01628 0.02126 AFIX 137 H24A 2 0.428468 0.069588 0.492396 -21.00000 -1.50000 H24B 2 0.338464 0.143169 0.437456 -21.00000 -1.50000 H24C 2 0.364254 0.164971 0.519491 -21.00000 -1.50000 AFIX 5 C25 1 0.515321 0.161606 0.324721 -21.00000 0.06148 0.03102 = 0.03924 -0.01250 -0.01597 0.01296 AFIX 137 H25A 2 0.552802 0.092641 0.353952 -21.00000 -1.50000 H25B 2 0.560789 0.204401 0.280351 -21.00000 -1.50000 H25C 2 0.465896 0.158603 0.292346 -21.00000 -1.50000 AFIX 5 C26 1 0.540165 0.212069 0.449292 -21.00000 0.08068 0.02750 = 0.09042 -0.01412 -0.05568 0.00539 AFIX 137 H26A 2 0.573601 0.142736 0.483195 -21.00000 -1.50000 H26B 2 0.507244 0.246916 0.492842 -21.00000 -1.50000 H26C 2 0.589085 0.249704 0.404117 -21.00000 -1.50000 AFIX 0 part 0 RESI 13 TBU part 0 ! ############################# C27 1 0.133450 0.955250 0.156978 11.00000 0.03314 0.01785 = 0.02410 -0.00459 0.00040 -0.00424 C28 1 0.201002 1.023204 0.083233 11.00000 0.04843 0.02056 = 0.03908 -0.00047 0.00973 -0.00450 AFIX 137 H28A 2 0.165269 1.094381 0.064263 11.00000 -1.50000 H28B 2 0.220784 1.002041 0.029476 11.00000 -1.50000 H28C 2 0.260180 1.016674 0.108769 11.00000 -1.50000 AFIX 0 C29 1 0.097162 0.996484 0.236032 11.00000 0.04094 0.02018 = 0.03172 -0.01004 -0.00069 -0.00549 AFIX 137 H29A 2 0.064045 1.068264 0.211540 11.00000 -1.50000 H29B 2 0.153865 0.990639 0.264607 11.00000 -1.50000 H29C 2 0.050378 0.956909 0.282489 11.00000 -1.50000 AFIX 0 C30 1 0.044083 0.960810 0.114727 11.00000 0.04510 0.02867 = 0.03413 -0.01014 -0.01400 0.00414 AFIX 137 H30A 2 0.008227 1.031715 0.091570 11.00000 -1.50000 H30B 2 -0.000234 0.918791 0.162103 11.00000 -1.50000 H30C 2 0.067208 0.935474 0.063536 11.00000 -1.50000 AFIX 0 C31 1 -0.016894 0.801483 0.583768 11.00000 0.02848 0.01781 = 0.02366 -0.00984 -0.00364 -0.00513 C32 1 0.062552 0.863645 0.526516 11.00000 0.03781 0.02586 = 0.03735 -0.01864 0.00296 -0.01297 AFIX 137 H32A 2 0.063011 0.913140 0.553491 11.00000 -1.50000 H32B 2 0.047882 0.899828 0.462821 11.00000 -1.50000 H32C 2 0.127633 0.817772 0.526574 11.00000 -1.50000 AFIX 0 C33 1 0.008044 0.745842 0.683224 11.00000 0.03930 0.02639 = 0.02904 -0.01351 -0.01059 -0.00411 AFIX 137 H33A 2 0.009466 0.795961 0.709107 11.00000 -1.50000 H33B 2 0.073068 0.699963 0.682678 11.00000 -1.50000 H33C 2 -0.042517 0.706160 0.721238 11.00000 -1.50000 AFIX 0 C34 1 -0.118349 0.874111 0.585399 11.00000 0.03286 0.01802 = 0.02897 -0.01231 -0.00257 -0.00271 AFIX 137 H34A 2 -0.115316 0.925155 0.609520 11.00000 -1.50000 H34B 2 -0.168780 0.835106 0.625238 11.00000 -1.50000 H34C 2 -0.135655 0.908392 0.522481 11.00000 -1.50000 AFIX 0 RESI 0 RESI 3 DCM C1 1 0.588174 0.156409 0.692264 11.00000 0.04116 0.05900 = 0.03952 -0.02132 -0.00141 -0.01445 AFIX 23 H1A 2 0.585092 0.160565 0.753402 11.00000 -1.20000 H1B 2 0.519932 0.178780 0.676301 11.00000 -1.20000 AFIX 0 CL2 3 0.633072 0.030438 0.699697 11.00000 0.08713 0.04515 = 0.09812 -0.00792 -0.02517 -0.01320 CL3 3 0.661814 0.238665 0.609629 11.00000 0.06442 0.06465 = 0.04982 -0.00880 -0.01393 -0.03371 RESI 0 RESI 4 DCM C1 1 0.009261 0.351262 0.807059 11.00000 0.04956 0.07934 = 0.03946 -0.02478 -0.00175 -0.01234 AFIX 23 H1A 2 0.045087 0.356102 0.744634 11.00000 -1.20000 H1B 2 -0.053074 0.328728 0.814637 11.00000 -1.20000 AFIX 0 CL2 3 0.082389 0.260364 0.890577 11.00000 0.04224 0.07003 = 0.06184 -0.02116 -0.00391 0.00230 CL3 3 -0.019045 0.471350 0.815924 11.00000 0.10619 0.04690 = 0.09885 0.00347 -0.01865 -0.02279 RESI 0 HKLF 4 REM KR1112_AsSw_a.res in P-1 REM wR2 = 0.171025, GooF = S = 1.07188, Restrained GooF = 1.09651 for all data REM R1 = 0.064267 for 10627 Fo > 4sig(Fo) and 0.067068 for all 11428 data REM 687 parameters refined using 413 restraints END WGHT 0.0805 3.2808 REM Highest difference peak 1.170, deepest hole -1.228, 1-sigma level 0.062 Q1 1 -0.0880 0.4670 0.8240 11.00000 0.05 1.17 Q2 1 0.5726 0.0405 0.6807 11.00000 0.05 0.88 Q3 1 0.2172 -0.3100 0.8251 11.00000 0.05 0.83 Q4 1 0.3180 -0.3489 0.9407 11.00000 0.05 0.79 Q5 1 0.0051 0.4626 0.8655 11.00000 0.05 0.78 Q6 1 0.6767 0.0463 0.6512 11.00000 0.05 0.70 Q7 1 0.0186 0.4456 0.7707 11.00000 0.05 0.68 Q8 1 0.1285 -0.2889 0.8905 11.00000 0.05 0.66 Q9 1 0.6934 0.1869 0.5809 11.00000 0.05 0.48 Q10 1 0.0846 0.3311 0.8718 11.00000 0.05 0.48 Q11 1 0.2993 -0.3343 0.8731 11.00000 0.05 0.46 Q12 1 0.3986 0.1320 0.4450 11.00000 0.05 0.45 Q13 1 0.4370 0.1406 0.3659 11.00000 0.05 0.43 Q14 1 0.5348 0.1550 0.3510 11.00000 0.05 0.42 Q15 1 0.3533 0.4797 0.5318 11.00000 0.05 0.41 Q16 1 0.2237 -0.3181 1.0100 11.00000 0.05 0.38 Q17 1 0.4553 0.2330 0.3919 11.00000 0.05 0.37 Q18 1 0.3802 0.4783 0.6848 11.00000 0.05 0.36 Q19 1 0.4990 0.1920 0.4827 11.00000 0.05 0.35 Q20 1 0.4362 0.1679 0.5107 11.00000 0.05 0.35 ; _shelx_res_checksum 26111 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1_1 C 0.29574(16) 0.35074(16) 0.68852(14) 0.0263(4) Uani 1 1 d . . . . . C2_1 C 0.23940(16) 0.31974(16) 0.64810(14) 0.0266(4) Uani 1 1 d . . . . . H2_1 H 0.205549 0.368890 0.598527 0.032 Uiso 1 1 calc R U . . . C3_1 C 0.23130(15) 0.21742(16) 0.67878(13) 0.0240(4) Uani 1 1 d . . . . . C4_1 C 0.17255(15) 0.18469(17) 0.63815(14) 0.0271(4) Uani 1 1 d . . . . . H4_1 H 0.138987 0.233163 0.588113 0.033 Uiso 1 1 calc R U . . . C5_1 C 0.16401(15) 0.08607(17) 0.66971(14) 0.0273(4) Uani 1 1 d . . . . . H5_1 H 0.122848 0.067255 0.642558 0.033 Uiso 1 1 calc R U . . . C6_1 C 0.21555(15) 0.00925(16) 0.74312(14) 0.0242(4) Uani 1 1 d . . . . . C7_1 C 0.20343(16) -0.09222(16) 0.78044(15) 0.0268(4) Uani 1 1 d . . . . . H7_1 H 0.161111 -0.111799 0.755112 0.032 Uiso 1 1 calc R U . . . C8_1 C 0.25147(14) -0.16455(15) 0.85316(14) 0.0261(4) Uani 1 1 d D . . . . C9_1 C 0.32064(15) -0.13597(15) 0.88403(14) 0.0238(4) Uani 1 1 d . . . . . H9_1 H 0.357282 -0.186145 0.931168 0.029 Uiso 1 1 calc R U . . . C10_1 C 0.33728(14) -0.03653(15) 0.84781(13) 0.0220(4) Uani 1 1 d . . . . . C11_1 C 0.40134(14) -0.00400(15) 0.88579(13) 0.0213(4) Uani 1 1 d . . . . . C12_1 C 0.48204(14) -0.07555(14) 0.93562(13) 0.0204(4) Uani 1 1 d . . . . . C13_1 C 0.53332(15) -0.16340(15) 0.91642(13) 0.0218(4) Uani 1 1 d . . . . . H13_1 H 0.511639 -0.179998 0.873099 0.026 Uiso 1 1 calc R U . . . C14_1 C 0.61545(14) -0.22712(14) 0.95934(13) 0.0211(4) Uani 1 1 d . . . . . C15_1 C 0.63803(14) -0.20924(14) 1.03135(13) 0.0204(4) Uani 1 1 d . . . . . H15_1 H 0.688128 -0.256914 1.066411 0.025 Uiso 1 1 calc R U . . . C16_1 C 0.58863(14) -0.12248(14) 1.05348(13) 0.0194(4) Uani 1 1 d . . . . . C17_1 C 0.51806(14) -0.04944(14) 0.99697(13) 0.0195(4) Uani 1 1 d . . . . . C18_1 C 0.38205(14) 0.09772(15) 0.87740(13) 0.0205(4) Uani 1 1 d . . . . . C19_1 C 0.33223(14) 0.17537(15) 0.80023(13) 0.0212(4) Uani 1 1 d . . . . . C20_1 C 0.34067(15) 0.27754(15) 0.76510(14) 0.0235(4) Uani 1 1 d . . . . . H20_1 H 0.378195 0.298365 0.794055 0.028 Uiso 1 1 calc R U . . . C21_1 C 0.28177(14) 0.14363(15) 0.75271(13) 0.0220(4) Uani 1 1 d . . . . . C22_1 C 0.27832(14) 0.03886(15) 0.78111(13) 0.0219(4) Uani 1 1 d . . . . . C23_1 C 0.31204(19) 0.46041(17) 0.65205(16) 0.0342(5) Uani 1 1 d . . . . . C24_1 C 0.2499(3) 0.5317(2) 0.5749(2) 0.0615(9) Uani 1 1 d . . . . . H24A_1 H 0.256622 0.602041 0.558512 0.092 Uiso 1 1 calc R U . . . H24B_1 H 0.180129 0.526876 0.596443 0.092 Uiso 1 1 calc R U . . . H24C_1 H 0.273199 0.511842 0.520537 0.092 Uiso 1 1 calc R U . . . C25_1 C 0.4221(2) 0.4600(2) 0.61641(19) 0.0467(6) Uani 1 1 d . . . . . H25A_1 H 0.433413 0.529607 0.593824 0.070 Uiso 1 1 calc R U . . . H25B_1 H 0.442197 0.433643 0.565793 0.070 Uiso 1 1 calc R U . . . H25C_1 H 0.461223 0.416321 0.666756 0.070 Uiso 1 1 calc R U . . . C26_1 C 0.2813(2) 0.50326(18) 0.73054(19) 0.0402(6) Uani 1 1 d . . . . . H26A_1 H 0.291692 0.573383 0.706618 0.060 Uiso 1 1 calc R U . . . H26B_1 H 0.321603 0.460999 0.780310 0.060 Uiso 1 1 calc R U . . . H26C_1 H 0.211136 0.502687 0.754669 0.060 Uiso 1 1 calc R U . . . C27_2 C 0.22987(12) -0.27325(11) 0.90483(11) 0.0318(5) Uani 0.136(4) 1 d DG U P A 1 C28_2 C 0.2897(2) -0.32881(19) 0.98602(18) 0.0878(15) Uani 0.136(4) 1 d DG U P A 1 H28A_2 H 0.257838 -0.383461 1.032745 0.132 Uiso 0.136(4) 1 calc R U P A 1 H28B_2 H 0.292366 -0.280469 1.013430 0.132 Uiso 0.136(4) 1 calc R U P A 1 H28C_2 H 0.357133 -0.358092 0.963892 0.132 Uiso 0.136(4) 1 calc R U P A 1 C29_2 C 0.11920(12) -0.2663(2) 0.9413(3) 0.0777(14) Uani 0.136(4) 1 d DG U P A 1 H29A_2 H 0.094216 -0.313144 0.925834 0.117 Uiso 0.136(4) 1 calc R U P A 1 H29B_2 H 0.083283 -0.196430 0.912688 0.117 Uiso 0.136(4) 1 calc R U P A 1 H29C_2 H 0.109219 -0.285051 1.008564 0.117 Uiso 0.136(4) 1 calc R U P A 1 C30_2 C 0.2597(3) -0.33208(19) 0.83884(17) 0.0648(11) Uani 0.136(4) 1 d DG U P A 1 H30A_2 H 0.235788 -0.396193 0.868401 0.097 Uiso 0.136(4) 1 calc R U P A 1 H30B_2 H 0.332073 -0.346867 0.823989 0.097 Uiso 0.136(4) 1 calc R U P A 1 H30C_2 H 0.230307 -0.290868 0.781851 0.097 Uiso 0.136(4) 1 calc R U P A 1 C27_20 C 0.22987(12) -0.27325(11) 0.90483(11) 0.0318(5) Uani 0.864(4) 1 d DG U P A 2 C28_20 C 0.1560(3) -0.2893(2) 0.8581(2) 0.0878(15) Uani 0.864(4) 1 d DG U P A 2 H28A_20 H 0.138571 -0.356151 0.893892 0.132 Uiso 0.864(4) 1 calc R U P A 2 H28B_20 H 0.186136 -0.286438 0.795306 0.132 Uiso 0.864(4) 1 calc R U P A 2 H28C_20 H 0.096109 -0.235773 0.854996 0.132 Uiso 0.864(4) 1 calc R U P A 2 C29_20 C 0.32651(17) -0.35181(15) 0.9028(2) 0.0777(14) Uani 0.864(4) 1 d DG U P A 2 H29A_20 H 0.312364 -0.420633 0.932133 0.117 Uiso 0.864(4) 1 calc R U P A 2 H29B_20 H 0.372125 -0.344566 0.936509 0.117 Uiso 0.864(4) 1 calc R U P A 2 H29C_20 H 0.356947 -0.340565 0.838533 0.117 Uiso 0.864(4) 1 calc R U P A 2 C30_20 C 0.1860(3) -0.2861(2) 1.00524(13) 0.0648(11) Uani 0.864(4) 1 d DG U P A 2 H30A_20 H 0.174389 -0.355583 1.038778 0.097 Uiso 0.864(4) 1 calc R U P A 2 H30B_20 H 0.123115 -0.237114 1.006582 0.097 Uiso 0.864(4) 1 calc R U P A 2 H30C_20 H 0.232470 -0.273759 1.034660 0.097 Uiso 0.864(4) 1 calc R U P A 2 C31 C 0.67961(15) -0.31115(15) 0.92368(14) 0.0245(4) Uani 1 1 d . . . . . C32 C 0.61492(17) -0.37588(17) 0.91681(17) 0.0324(5) Uani 1 1 d . . . . . H32A H 0.657128 -0.429713 0.895068 0.049 Uiso 1 1 calc R U . . . H32B H 0.567913 -0.332510 0.873106 0.049 Uiso 1 1 calc R U . . . H32C H 0.578346 -0.406809 0.977856 0.049 Uiso 1 1 calc R U . . . C33 C 0.75847(17) -0.38134(17) 0.98534(17) 0.0321(5) Uani 1 1 d . . . . . H33A H 0.795543 -0.435199 0.961454 0.048 Uiso 1 1 calc R U . . . H33B H 0.726327 -0.412150 1.048566 0.048 Uiso 1 1 calc R U . . . H33C H 0.804062 -0.341647 0.985504 0.048 Uiso 1 1 calc R U . . . C34 C 0.7326(2) -0.25975(19) 0.82658(17) 0.0398(6) Uani 1 1 d . . . . . H34A H 0.772896 -0.312090 0.802005 0.060 Uiso 1 1 calc R U . . . H34B H 0.775539 -0.219326 0.830125 0.060 Uiso 1 1 calc R U . . . H34C H 0.683311 -0.215045 0.785658 0.060 Uiso 1 1 calc R U . . . C1_11 C 0.40861(15) 0.31861(15) 0.35395(14) 0.0247(4) Uani 1 1 d D . . . . C2_11 C 0.45960(15) 0.38921(16) 0.28479(15) 0.0261(4) Uani 1 1 d . . . . . H2_11 H 0.526277 0.366742 0.261461 0.031 Uiso 1 1 calc R U . . . C3_11 C 0.41532(15) 0.49278(15) 0.24845(14) 0.0230(4) Uani 1 1 d . . . . . C4_11 C 0.46726(15) 0.56685(16) 0.17708(14) 0.0267(4) Uani 1 1 d . . . . . H4_11 H 0.532934 0.544935 0.151158 0.032 Uiso 1 1 calc R U . . . C5_11 C 0.42443(15) 0.66740(16) 0.14598(14) 0.0258(4) Uani 1 1 d . . . . . H5_11 H 0.459686 0.714188 0.097151 0.031 Uiso 1 1 calc R U . . . C6_11 C 0.32666(15) 0.70432(15) 0.18564(13) 0.0224(4) Uani 1 1 d . . . . . C7_11 C 0.28213(15) 0.80846(15) 0.15563(13) 0.0237(4) Uani 1 1 d . . . . . H7_11 H 0.317622 0.856012 0.108049 0.028 Uiso 1 1 calc R U . . . C8_11 C 0.18748(15) 0.84337(15) 0.19395(13) 0.0229(4) Uani 1 1 d . . . . . C9_11 C 0.13902(15) 0.77242(14) 0.26822(13) 0.0213(4) Uani 1 1 d . . . . . H9_11 H 0.074816 0.795958 0.295830 0.026 Uiso 1 1 calc R U . . . C10_11 C 0.18164(14) 0.66849(14) 0.30306(13) 0.0200(4) Uani 1 1 d . . . . . C11_11 C 0.13068(14) 0.59320(14) 0.37821(13) 0.0192(4) Uani 1 1 d . . . . . C12_11 C 0.05307(14) 0.61913(14) 0.44800(13) 0.0187(4) Uani 1 1 d . . . . . C13_11 C 0.04697(14) 0.70369(14) 0.47188(13) 0.0195(4) Uani 1 1 d . . . . . H13_11 H 0.089702 0.750083 0.436737 0.023 Uiso 1 1 calc R U . . . C14_11 C -0.02022(14) 0.72105(14) 0.54584(13) 0.0198(4) Uani 1 1 d . . . . . C15_11 C -0.09143(14) 0.66043(14) 0.58886(13) 0.0200(4) Uani 1 1 d . . . . . H15_11 H -0.142831 0.677089 0.633829 0.024 Uiso 1 1 calc R U . . . C16_11 C -0.08883(14) 0.57562(14) 0.56728(13) 0.0189(4) Uani 1 1 d . . . . . C17_11 C -0.00857(14) 0.54871(13) 0.50413(13) 0.0182(4) Uani 1 1 d . . . . . C18_11 C 0.15907(14) 0.49165(14) 0.38464(13) 0.0195(4) Uani 1 1 d . . . . . C19_11 C 0.26013(14) 0.45461(14) 0.34756(13) 0.0200(4) Uani 1 1 d . . . . . C20_11 C 0.30832(15) 0.35190(15) 0.38209(13) 0.0223(4) Uani 1 1 d . . . . . H20_11 H 0.271459 0.303333 0.426127 0.027 Uiso 1 1 calc R U . . . C21_11 C 0.31669(14) 0.52677(14) 0.28427(13) 0.0204(4) Uani 1 1 d . . . . . C22_11 C 0.27439(14) 0.63329(14) 0.25696(13) 0.0205(4) Uani 1 1 d . . . . . C23_12 C 0.4597(2) 0.20725(15) 0.40484(19) 0.0293(5) Uani 0.542(3) 1 d DG U P B 1 C24_12 C 0.5634(3) 0.1808(4) 0.3544(3) 0.0694(15) Uani 0.542(3) 1 d G U P B 1 H24A_12 H 0.585943 0.106534 0.375499 0.104 Uiso 0.542(3) 1 calc R U P B 1 H24B_12 H 0.609423 0.210939 0.367737 0.104 Uiso 0.542(3) 1 calc R U P B 1 H24C_12 H 0.561294 0.207948 0.287599 0.104 Uiso 0.542(3) 1 calc R U P B 1 C25_12 C 0.4678(4) 0.1966(3) 0.5026(2) 0.0471(9) Uani 0.542(3) 1 d G U P B 1 H25A_12 H 0.503543 0.127834 0.534879 0.071 Uiso 0.542(3) 1 calc R U P B 1 H25B_12 H 0.401138 0.208357 0.536537 0.071 Uiso 0.542(3) 1 calc R U P B 1 H25C_12 H 0.503726 0.246938 0.498969 0.071 Uiso 0.542(3) 1 calc R U P B 1 C26_12 C 0.3967(4) 0.1345(3) 0.4105(4) 0.0642(12) Uani 0.542(3) 1 d G U P B 1 H26A_12 H 0.425698 0.064634 0.447513 0.096 Uiso 0.542(3) 1 calc R U P B 1 H26B_12 H 0.394762 0.138375 0.348033 0.096 Uiso 0.542(3) 1 calc R U P B 1 H26C_12 H 0.329134 0.153979 0.439542 0.096 Uiso 0.542(3) 1 calc R U P B 1 C23_120 C 0.4630(3) 0.20715(17) 0.3989(2) 0.0293(5) Uani 0.458(3) 1 d DG U P B 2 C24_120 C 0.3922(4) 0.1402(4) 0.4683(4) 0.0694(15) Uani 0.458(3) 1 d G U P B 2 H24A_120 H 0.428468 0.069588 0.492396 0.104 Uiso 0.458(3) 1 calc R U P B 2 H24B_120 H 0.338464 0.143169 0.437456 0.104 Uiso 0.458(3) 1 calc R U P B 2 H24C_120 H 0.364254 0.164971 0.519491 0.104 Uiso 0.458(3) 1 calc R U P B 2 C25_120 C 0.5153(4) 0.1616(4) 0.3247(3) 0.0471(9) Uani 0.458(3) 1 d G U P B 2 H25A_120 H 0.552802 0.092641 0.353952 0.071 Uiso 0.458(3) 1 calc R U P B 2 H25B_120 H 0.560789 0.204401 0.280351 0.071 Uiso 0.458(3) 1 calc R U P B 2 H25C_120 H 0.465896 0.158603 0.292346 0.071 Uiso 0.458(3) 1 calc R U P B 2 C26_120 C 0.5402(5) 0.2121(4) 0.4493(4) 0.0642(12) Uani 0.458(3) 1 d G U P B 2 H26A_120 H 0.573601 0.142736 0.483195 0.096 Uiso 0.458(3) 1 calc R U P B 2 H26B_120 H 0.507244 0.246916 0.492842 0.096 Uiso 0.458(3) 1 calc R U P B 2 H26C_120 H 0.589085 0.249704 0.404117 0.096 Uiso 0.458(3) 1 calc R U P B 2 C27_13 C 0.13345(16) 0.95525(15) 0.15698(14) 0.0270(4) Uani 1 1 d . . . . . C28_13 C 0.2010(2) 1.02320(17) 0.08323(18) 0.0427(6) Uani 1 1 d . . . . . H28A_13 H 0.165269 1.094381 0.064263 0.064 Uiso 1 1 calc R U . . . H28B_13 H 0.220784 1.002041 0.029476 0.064 Uiso 1 1 calc R U . . . H28C_13 H 0.260180 1.016674 0.108769 0.064 Uiso 1 1 calc R U . . . C29_13 C 0.09716(18) 0.99648(16) 0.23603(16) 0.0317(5) Uani 1 1 d . . . . . H29A_13 H 0.064045 1.068264 0.211540 0.047 Uiso 1 1 calc R U . . . H29B_13 H 0.153865 0.990639 0.264607 0.047 Uiso 1 1 calc R U . . . H29C_13 H 0.050378 0.956909 0.282489 0.047 Uiso 1 1 calc R U . . . C30_13 C 0.04408(19) 0.96081(18) 0.11473(17) 0.0373(5) Uani 1 1 d . . . . . H30A_13 H 0.008227 1.031715 0.091570 0.056 Uiso 1 1 calc R U . . . H30B_13 H -0.000234 0.918791 0.162103 0.056 Uiso 1 1 calc R U . . . H30C_13 H 0.067208 0.935474 0.063536 0.056 Uiso 1 1 calc R U . . . C31_13 C -0.01689(15) 0.80148(14) 0.58377(14) 0.0224(4) Uani 1 1 d . . . . . C32_13 C 0.06255(18) 0.86365(17) 0.52652(16) 0.0314(5) Uani 1 1 d . . . . . H32A_13 H 0.063011 0.913140 0.553491 0.047 Uiso 1 1 calc R U . . . H32B_13 H 0.047882 0.899828 0.462821 0.047 Uiso 1 1 calc R U . . . H32C_13 H 0.127633 0.817772 0.526574 0.047 Uiso 1 1 calc R U . . . C33_13 C 0.00804(18) 0.74584(16) 0.68322(15) 0.0299(5) Uani 1 1 d . . . . . H33A_13 H 0.009466 0.795961 0.709107 0.045 Uiso 1 1 calc R U . . . H33B_13 H 0.073068 0.699963 0.682678 0.045 Uiso 1 1 calc R U . . . H33C_13 H -0.042517 0.706160 0.721238 0.045 Uiso 1 1 calc R U . . . C34_13 C -0.11835(16) 0.87411(15) 0.58540(15) 0.0262(4) Uani 1 1 d . . . . . H34A_13 H -0.115316 0.925155 0.609520 0.039 Uiso 1 1 calc R U . . . H34B_13 H -0.168780 0.835106 0.625238 0.039 Uiso 1 1 calc R U . . . H34C_13 H -0.135655 0.908392 0.522481 0.039 Uiso 1 1 calc R U . . . C1_3 C 0.5882(2) 0.1564(2) 0.69226(19) 0.0452(6) Uani 1 1 d . . . . . H1A_3 H 0.585092 0.160565 0.753402 0.054 Uiso 1 1 calc R U . . . H1B_3 H 0.519932 0.178780 0.676301 0.054 Uiso 1 1 calc R U . . . Cl2_3 Cl 0.63307(8) 0.03044(7) 0.69970(8) 0.0805(3) Uani 1 1 d . . . . . Cl3_3 Cl 0.66181(6) 0.23866(6) 0.60963(5) 0.0580(2) Uani 1 1 d . . . . . C1_4 C 0.0093(2) 0.3513(3) 0.8071(2) 0.0560(8) Uani 1 1 d . . . . . H1A_4 H 0.045087 0.356102 0.744634 0.067 Uiso 1 1 calc R U . . . H1B_4 H -0.053074 0.328728 0.814637 0.067 Uiso 1 1 calc R U . . . Cl2_4 Cl 0.08239(6) 0.26036(7) 0.89058(6) 0.0624(2) Uani 1 1 d . . . . . Cl3_4 Cl -0.01904(9) 0.47135(7) 0.81592(9) 0.0914(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1_1 0.0280(10) 0.0240(10) 0.0223(9) -0.0034(8) -0.0047(8) -0.0048(8) C2_1 0.0289(10) 0.0253(10) 0.0201(9) -0.0017(8) -0.0078(8) -0.0031(8) C3_1 0.0230(9) 0.0265(10) 0.0198(9) -0.0073(8) -0.0028(7) -0.0027(8) C4_1 0.0257(10) 0.0298(11) 0.0226(10) -0.0057(8) -0.0075(8) -0.0027(8) C5_1 0.0245(10) 0.0339(11) 0.0252(10) -0.0106(9) -0.0070(8) -0.0053(8) C6_1 0.0225(9) 0.0262(10) 0.0233(9) -0.0103(8) -0.0042(8) -0.0012(8) C7_1 0.0265(10) 0.0282(10) 0.0302(10) -0.0149(9) -0.0071(8) -0.0033(8) C8_1 0.0286(10) 0.0230(10) 0.0288(10) -0.0129(8) -0.0057(8) -0.0014(8) C9_1 0.0251(10) 0.0214(9) 0.0245(9) -0.0099(8) -0.0066(8) 0.0008(8) C10_1 0.0216(9) 0.0224(9) 0.0213(9) -0.0103(8) -0.0024(7) -0.0001(7) C11_1 0.0215(9) 0.0214(9) 0.0191(9) -0.0074(7) -0.0026(7) -0.0017(7) C12_1 0.0206(9) 0.0190(9) 0.0184(9) -0.0049(7) -0.0016(7) -0.0028(7) C13_1 0.0240(9) 0.0209(9) 0.0196(9) -0.0073(7) -0.0037(7) -0.0026(7) C14_1 0.0222(9) 0.0177(9) 0.0209(9) -0.0060(7) -0.0013(7) -0.0030(7) C15_1 0.0198(9) 0.0179(9) 0.0197(9) -0.0032(7) -0.0029(7) -0.0030(7) C16_1 0.0188(9) 0.0187(9) 0.0184(8) -0.0045(7) -0.0016(7) -0.0041(7) C17_1 0.0184(8) 0.0186(9) 0.0181(8) -0.0046(7) -0.0008(7) -0.0029(7) C18_1 0.0190(9) 0.0205(9) 0.0194(9) -0.0058(7) -0.0020(7) -0.0023(7) C19_1 0.0193(9) 0.0219(9) 0.0196(9) -0.0067(8) -0.0020(7) -0.0014(7) C20_1 0.0239(9) 0.0227(10) 0.0217(9) -0.0057(8) -0.0052(8) -0.0033(8) C21_1 0.0201(9) 0.0235(10) 0.0196(9) -0.0072(8) -0.0017(7) -0.0017(7) C22_1 0.0208(9) 0.0237(10) 0.0200(9) -0.0089(8) -0.0023(7) -0.0014(7) C23_1 0.0432(13) 0.0253(11) 0.0303(11) 0.0009(9) -0.0131(10) -0.0109(9) C24_1 0.095(3) 0.0317(14) 0.0565(18) 0.0117(12) -0.0469(18) -0.0233(15) C25_1 0.0584(17) 0.0466(15) 0.0356(13) -0.0087(11) 0.0023(12) -0.0281(13) C26_1 0.0454(14) 0.0258(11) 0.0462(14) -0.0080(10) -0.0125(11) -0.0046(10) C27_2 0.0368(11) 0.0227(10) 0.0395(12) -0.0132(9) -0.0101(9) -0.0045(9) C28_2 0.137(4) 0.0411(19) 0.103(3) 0.0055(19) -0.078(3) -0.042(2) C29_2 0.056(2) 0.0219(14) 0.116(3) -0.0079(17) 0.025(2) -0.0034(14) C30_2 0.091(3) 0.055(2) 0.0581(19) -0.0297(16) 0.0293(18) -0.0475(19) C27_20 0.0368(11) 0.0227(10) 0.0395(12) -0.0132(9) -0.0101(9) -0.0045(9) C28_20 0.137(4) 0.0411(19) 0.103(3) 0.0055(19) -0.078(3) -0.042(2) C29_20 0.056(2) 0.0219(14) 0.116(3) -0.0079(17) 0.025(2) -0.0034(14) C30_20 0.091(3) 0.055(2) 0.0581(19) -0.0297(16) 0.0293(18) -0.0475(19) C31 0.0256(10) 0.0211(9) 0.0243(10) -0.0096(8) -0.0032(8) 0.0011(8) C32 0.0341(11) 0.0284(11) 0.0403(12) -0.0203(10) -0.0112(10) 0.0022(9) C33 0.0326(11) 0.0251(10) 0.0404(12) -0.0174(9) -0.0128(10) 0.0061(9) C34 0.0419(13) 0.0323(12) 0.0318(12) -0.0116(10) 0.0087(10) 0.0018(10) C1_11 0.0274(10) 0.0217(10) 0.0248(10) -0.0112(8) -0.0045(8) 0.0006(8) C2_11 0.0219(9) 0.0270(10) 0.0281(10) -0.0130(8) -0.0023(8) 0.0007(8) C3_11 0.0225(9) 0.0245(10) 0.0229(9) -0.0101(8) -0.0032(7) -0.0037(8) C4_11 0.0220(9) 0.0301(11) 0.0264(10) -0.0106(9) -0.0001(8) -0.0048(8) C5_11 0.0249(10) 0.0267(10) 0.0239(10) -0.0070(8) 0.0003(8) -0.0086(8) C6_11 0.0246(10) 0.0225(9) 0.0210(9) -0.0082(8) -0.0022(7) -0.0065(8) C7_11 0.0281(10) 0.0219(9) 0.0202(9) -0.0054(8) -0.0008(8) -0.0092(8) C8_11 0.0292(10) 0.0185(9) 0.0210(9) -0.0062(7) -0.0037(8) -0.0058(8) C9_11 0.0250(9) 0.0185(9) 0.0203(9) -0.0073(7) -0.0020(7) -0.0045(7) C10_11 0.0233(9) 0.0184(9) 0.0196(9) -0.0075(7) -0.0032(7) -0.0052(7) C11_11 0.0218(9) 0.0166(9) 0.0191(9) -0.0064(7) -0.0038(7) -0.0033(7) C12_11 0.0214(9) 0.0150(8) 0.0181(8) -0.0047(7) -0.0044(7) -0.0019(7) C13_11 0.0230(9) 0.0139(8) 0.0200(9) -0.0048(7) -0.0037(7) -0.0030(7) C14_11 0.0250(9) 0.0135(8) 0.0209(9) -0.0062(7) -0.0058(7) -0.0015(7) C15_11 0.0238(9) 0.0155(8) 0.0186(9) -0.0060(7) -0.0026(7) -0.0014(7) C16_11 0.0228(9) 0.0144(8) 0.0179(8) -0.0046(7) -0.0045(7) -0.0017(7) C17_11 0.0218(9) 0.0144(9) 0.0178(8) -0.0052(7) -0.0047(7) -0.0021(7) C18_11 0.0235(9) 0.0169(9) 0.0174(8) -0.0063(7) -0.0030(7) -0.0029(7) C19_11 0.0233(9) 0.0186(9) 0.0194(9) -0.0090(7) -0.0034(7) -0.0027(7) C20_11 0.0260(10) 0.0180(9) 0.0221(9) -0.0083(7) -0.0021(7) -0.0030(7) C21_11 0.0229(9) 0.0198(9) 0.0199(9) -0.0087(7) -0.0039(7) -0.0033(7) C22_11 0.0234(9) 0.0199(9) 0.0201(9) -0.0082(7) -0.0034(7) -0.0053(7) C23_12 0.0313(11) 0.0221(10) 0.0299(11) -0.0094(8) -0.0071(9) 0.0045(8) C24_12 0.054(2) 0.035(2) 0.061(3) 0.0089(19) 0.016(2) 0.0213(17) C25_12 0.061(2) 0.0310(17) 0.0392(18) -0.0125(15) -0.0160(17) 0.0130(16) C26_12 0.081(3) 0.0275(17) 0.090(3) -0.014(2) -0.056(3) 0.0054(18) C23_120 0.0313(11) 0.0221(10) 0.0299(11) -0.0094(8) -0.0071(9) 0.0045(8) C24_120 0.054(2) 0.035(2) 0.061(3) 0.0089(19) 0.016(2) 0.0213(17) C25_120 0.061(2) 0.0310(17) 0.0392(18) -0.0125(15) -0.0160(17) 0.0130(16) C26_120 0.081(3) 0.0275(17) 0.090(3) -0.014(2) -0.056(3) 0.0054(18) C27_13 0.0331(11) 0.0178(9) 0.0241(10) -0.0046(8) 0.0004(8) -0.0042(8) C28_13 0.0484(14) 0.0206(11) 0.0391(13) -0.0005(10) 0.0097(11) -0.0045(10) C29_13 0.0409(12) 0.0202(10) 0.0317(11) -0.0100(9) -0.0007(9) -0.0055(9) C30_13 0.0451(14) 0.0287(11) 0.0341(12) -0.0101(10) -0.0140(10) 0.0041(10) C31_13 0.0285(10) 0.0178(9) 0.0237(9) -0.0098(8) -0.0036(8) -0.0051(8) C32_13 0.0378(12) 0.0259(10) 0.0374(12) -0.0186(9) 0.0030(9) -0.0130(9) C33_13 0.0393(12) 0.0264(10) 0.0290(11) -0.0135(9) -0.0106(9) -0.0041(9) C34_13 0.0329(11) 0.0180(9) 0.0290(10) -0.0123(8) -0.0026(8) -0.0027(8) C1_3 0.0412(14) 0.0590(17) 0.0395(14) -0.0213(12) -0.0014(11) -0.0145(12) Cl2_3 0.0871(7) 0.0452(4) 0.0981(7) -0.0079(4) -0.0252(6) -0.0132(4) Cl3_3 0.0644(5) 0.0646(5) 0.0498(4) -0.0088(3) -0.0139(3) -0.0337(4) C1_4 0.0496(16) 0.079(2) 0.0395(15) -0.0248(15) -0.0018(12) -0.0123(15) Cl2_4 0.0422(4) 0.0700(5) 0.0618(5) -0.0212(4) -0.0039(3) 0.0023(3) Cl3_4 0.1062(8) 0.0469(5) 0.0989(8) 0.0035(5) -0.0186(6) -0.0228(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 1 0 0.0799 -1 1 -1 0.0889 0 0 -1 0.0647 1 0 -1 0.0286 -1 0 1 0.0350 0 1 1 0.0406 0 -1 -1 0.0414 1 0 1 0.0683 -1 0 -1 0.0674 2 1 -1 0.0279 -1 -1 0 0.0404 2 1 1 0.0455 -1 -1 -2 0.0564 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2_1 C1_1 C20_1 118.12(19) . . ? C2_1 C1_1 C23_1 122.66(18) . . ? C20_1 C1_1 C23_1 119.21(19) . . ? C1_1 C2_1 C3_1 121.51(18) . . ? C1_1 C2_1 H2_1 119.2 . . ? C3_1 C2_1 H2_1 119.2 . . ? C2_1 C3_1 C21_1 119.51(19) . . ? C2_1 C3_1 C4_1 121.99(18) . . ? C21_1 C3_1 C4_1 118.49(19) . . ? C5_1 C4_1 C3_1 121.25(19) . . ? C5_1 C4_1 H4_1 119.4 . . ? C3_1 C4_1 H4_1 119.4 . . ? C4_1 C5_1 C6_1 121.65(19) . . ? C4_1 C5_1 H5_1 119.2 . . ? C6_1 C5_1 H5_1 119.2 . . ? C7_1 C6_1 C22_1 119.26(18) . . ? C7_1 C6_1 C5_1 122.60(19) . . ? C22_1 C6_1 C5_1 118.09(19) . . ? C8_1 C7_1 C6_1 121.76(19) . . ? C8_1 C7_1 H7_1 119.1 . . ? C6_1 C7_1 H7_1 119.1 . . ? C7_1 C8_1 C9_1 118.00(19) . . ? C7_1 C8_1 C27_20 123.43(16) . . ? C9_1 C8_1 C27_20 118.51(15) . . ? C7_1 C8_1 C27_2 123.43(16) . . ? C9_1 C8_1 C27_2 118.51(15) . . ? C10_1 C9_1 C8_1 122.40(18) . . ? C10_1 C9_1 H9_1 118.8 . . ? C8_1 C9_1 H9_1 118.8 . . ? C9_1 C10_1 C22_1 118.22(18) . . ? C9_1 C10_1 C11_1 122.60(18) . . ? C22_1 C10_1 C11_1 118.48(18) . . ? C18_1 C11_1 C12_1 119.05(18) . . ? C18_1 C11_1 C10_1 118.78(17) . . ? C12_1 C11_1 C10_1 122.12(17) . . ? C13_1 C12_1 C17_1 118.35(17) . . ? C13_1 C12_1 C11_1 122.23(18) . . ? C17_1 C12_1 C11_1 118.94(17) . . ? C14_1 C13_1 C12_1 121.76(18) . . ? C14_1 C13_1 H13_1 119.1 . . ? C12_1 C13_1 H13_1 119.1 . . ? C15_1 C14_1 C13_1 118.15(17) . . ? C15_1 C14_1 C31 122.38(17) . . ? C13_1 C14_1 C31 119.42(17) . . ? C14_1 C15_1 C16_1 121.75(17) . . ? C14_1 C15_1 H15_1 119.1 . . ? C16_1 C15_1 H15_1 119.1 . . ? C15_1 C16_1 C17_1 118.16(17) . . ? C15_1 C16_1 C18_1 122.28(17) . 2_657 ? C17_1 C16_1 C18_1 118.89(17) . 2_657 ? C12_1 C17_1 C16_1 119.62(17) . . ? C12_1 C17_1 C17_1 119.9(2) . 2_657 ? C16_1 C17_1 C17_1 120.4(2) . 2_657 ? C11_1 C18_1 C16_1 118.60(17) . 2_657 ? C11_1 C18_1 C19_1 118.72(17) . . ? C16_1 C18_1 C19_1 122.68(17) 2_657 . ? C20_1 C19_1 C21_1 118.23(18) . . ? C20_1 C19_1 C18_1 123.01(18) . . ? C21_1 C19_1 C18_1 118.42(17) . . ? C19_1 C20_1 C1_1 122.56(19) . . ? C19_1 C20_1 H20_1 118.7 . . ? C1_1 C20_1 H20_1 118.7 . . ? C3_1 C21_1 C19_1 119.63(18) . . ? C3_1 C21_1 C22_1 119.94(18) . . ? C19_1 C21_1 C22_1 120.38(17) . . ? C10_1 C22_1 C6_1 119.58(18) . . ? C10_1 C22_1 C21_1 120.22(18) . . ? C6_1 C22_1 C21_1 120.21(18) . . ? C25_1 C23_1 C24_1 109.9(2) . . ? C25_1 C23_1 C1_1 108.9(2) . . ? C24_1 C23_1 C1_1 112.1(2) . . ? C25_1 C23_1 C26_1 108.8(2) . . ? C24_1 C23_1 C26_1 107.1(2) . . ? C1_1 C23_1 C26_1 109.99(19) . . ? C23_1 C24_1 H24A_1 109.5 . . ? C23_1 C24_1 H24B_1 109.5 . . ? H24A_1 C24_1 H24B_1 109.5 . . ? C23_1 C24_1 H24C_1 109.5 . . ? H24A_1 C24_1 H24C_1 109.5 . . ? H24B_1 C24_1 H24C_1 109.5 . . ? C23_1 C25_1 H25A_1 109.5 . . ? C23_1 C25_1 H25B_1 109.5 . . ? H25A_1 C25_1 H25B_1 109.5 . . ? C23_1 C25_1 H25C_1 109.5 . . ? H25A_1 C25_1 H25C_1 109.5 . . ? H25B_1 C25_1 H25C_1 109.5 . . ? C23_1 C26_1 H26A_1 109.5 . . ? C23_1 C26_1 H26B_1 109.5 . . ? H26A_1 C26_1 H26B_1 109.5 . . ? C23_1 C26_1 H26C_1 109.5 . . ? H26A_1 C26_1 H26C_1 109.5 . . ? H26B_1 C26_1 H26C_1 109.5 . . ? C28_2 C27_2 C29_2 109.5 . . ? C28_2 C27_2 C30_2 109.5 . . ? C29_2 C27_2 C30_2 109.5 . . ? C28_2 C27_2 C8_1 109.10(7) . . ? C29_2 C27_2 C8_1 109.57(7) . . ? C30_2 C27_2 C8_1 109.74(7) . . ? C27_2 C28_2 H28A_2 109.5 . . ? C27_2 C28_2 H28B_2 109.5 . . ? H28A_2 C28_2 H28B_2 109.5 . . ? C27_2 C28_2 H28C_2 109.5 . . ? H28A_2 C28_2 H28C_2 109.5 . . ? H28B_2 C28_2 H28C_2 109.5 . . ? C27_2 C29_2 H29A_2 109.5 . . ? C27_2 C29_2 H29B_2 109.5 . . ? H29A_2 C29_2 H29B_2 109.5 . . ? C27_2 C29_2 H29C_2 109.5 . . ? H29A_2 C29_2 H29C_2 109.5 . . ? H29B_2 C29_2 H29C_2 109.5 . . ? C27_2 C30_2 H30A_2 109.5 . . ? C27_2 C30_2 H30B_2 109.5 . . ? H30A_2 C30_2 H30B_2 109.5 . . ? C27_2 C30_2 H30C_2 109.5 . . ? H30A_2 C30_2 H30C_2 109.5 . . ? H30B_2 C30_2 H30C_2 109.5 . . ? C28_20 C27_20 C30_20 109.5 . . ? C28_20 C27_20 C29_20 109.5 . . ? C30_20 C27_20 C29_20 109.5 . . ? C28_20 C27_20 C8_1 109.84(7) . . ? C30_20 C27_20 C8_1 109.20(7) . . ? C29_20 C27_20 C8_1 109.37(7) . . ? C27_20 C28_20 H28A_20 109.5 . . ? C27_20 C28_20 H28B_20 109.5 . . ? H28A_20 C28_20 H28B_20 109.5 . . ? C27_20 C28_20 H28C_20 109.5 . . ? H28A_20 C28_20 H28C_20 109.5 . . ? H28B_20 C28_20 H28C_20 109.5 . . ? C27_20 C29_20 H29A_20 109.5 . . ? C27_20 C29_20 H29B_20 109.5 . . ? H29A_20 C29_20 H29B_20 109.5 . . ? C27_20 C29_20 H29C_20 109.5 . . ? H29A_20 C29_20 H29C_20 109.5 . . ? H29B_20 C29_20 H29C_20 109.5 . . ? C27_20 C30_20 H30A_20 109.5 . . ? C27_20 C30_20 H30B_20 109.5 . . ? H30A_20 C30_20 H30B_20 109.5 . . ? C27_20 C30_20 H30C_20 109.5 . . ? H30A_20 C30_20 H30C_20 109.5 . . ? H30B_20 C30_20 H30C_20 109.5 . . ? C33 C31 C32 108.83(17) . . ? C33 C31 C34 108.14(19) . . ? C32 C31 C34 108.55(19) . . ? C33 C31 C14_1 112.40(17) . . ? C32 C31 C14_1 110.63(17) . . ? C34 C31 C14_1 108.18(17) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C2_11 C1_11 C20_11 118.06(18) . . ? C2_11 C1_11 C23_120 120.2(2) . . ? C20_11 C1_11 C23_120 121.7(2) . . ? C2_11 C1_11 C23_12 122.7(2) . . ? C20_11 C1_11 C23_12 119.1(2) . . ? C1_11 C2_11 C3_11 121.78(19) . . ? C1_11 C2_11 H2_11 119.1 . . ? C3_11 C2_11 H2_11 119.1 . . ? C2_11 C3_11 C21_11 119.23(18) . . ? C2_11 C3_11 C4_11 122.43(19) . . ? C21_11 C3_11 C4_11 118.32(18) . . ? C5_11 C4_11 C3_11 121.38(19) . . ? C5_11 C4_11 H4_11 119.3 . . ? C3_11 C4_11 H4_11 119.3 . . ? C4_11 C5_11 C6_11 121.13(19) . . ? C4_11 C5_11 H5_11 119.4 . . ? C6_11 C5_11 H5_11 119.4 . . ? C7_11 C6_11 C22_11 119.49(18) . . ? C7_11 C6_11 C5_11 121.84(18) . . ? C22_11 C6_11 C5_11 118.67(18) . . ? C8_11 C7_11 C6_11 121.45(18) . . ? C8_11 C7_11 H7_11 119.3 . . ? C6_11 C7_11 H7_11 119.3 . . ? C7_11 C8_11 C9_11 118.17(18) . . ? C7_11 C8_11 C27_13 122.58(18) . . ? C9_11 C8_11 C27_13 119.23(18) . . ? C10_11 C9_11 C8_11 122.57(18) . . ? C10_11 C9_11 H9_11 118.7 . . ? C8_11 C9_11 H9_11 118.7 . . ? C9_11 C10_11 C22_11 118.05(17) . . ? C9_11 C10_11 C11_11 123.17(17) . . ? C22_11 C10_11 C11_11 118.46(17) . . ? C18_11 C11_11 C12_11 118.44(17) . . ? C18_11 C11_11 C10_11 118.55(17) . . ? C12_11 C11_11 C10_11 122.99(16) . . ? C13_11 C12_11 C17_11 117.97(17) . . ? C13_11 C12_11 C11_11 122.16(17) . . ? C17_11 C12_11 C11_11 119.09(16) . . ? C14_11 C13_11 C12_11 121.63(17) . . ? C14_11 C13_11 H13_11 119.2 . . ? C12_11 C13_11 H13_11 119.2 . . ? C13_11 C14_11 C15_11 118.42(17) . . ? C13_11 C14_11 C31_13 122.69(17) . . ? C15_11 C14_11 C31_13 118.86(17) . . ? C14_11 C15_11 C16_11 121.60(17) . . ? C14_11 C15_11 H15_11 119.2 . . ? C16_11 C15_11 H15_11 119.2 . . ? C15_11 C16_11 C17_11 118.28(17) . . ? C15_11 C16_11 C18_11 122.17(17) . 2_566 ? C17_11 C16_11 C18_11 119.16(16) . 2_566 ? C16_11 C17_11 C12_11 119.88(16) . . ? C16_11 C17_11 C17_11 119.7(2) . 2_566 ? C12_11 C17_11 C17_11 120.4(2) . 2_566 ? C11_11 C18_11 C16_11 119.04(17) . 2_566 ? C11_11 C18_11 C19_11 118.93(17) . . ? C16_11 C18_11 C19_11 121.93(16) 2_566 . ? C20_11 C19_11 C21_11 118.26(18) . . ? C20_11 C19_11 C18_11 122.45(17) . . ? C21_11 C19_11 C18_11 118.61(17) . . ? C1_11 C20_11 C19_11 122.35(18) . . ? C1_11 C20_11 H20_11 118.8 . . ? C19_11 C20_11 H20_11 118.8 . . ? C3_11 C21_11 C19_11 119.65(17) . . ? C3_11 C21_11 C22_11 120.19(18) . . ? C19_11 C21_11 C22_11 120.16(17) . . ? C6_11 C22_11 C10_11 119.79(17) . . ? C6_11 C22_11 C21_11 119.87(18) . . ? C10_11 C22_11 C21_11 120.30(17) . . ? C25_12 C23_12 C26_12 109.5 . . ? C25_12 C23_12 C24_12 109.5 . . ? C26_12 C23_12 C24_12 109.5 . . ? C25_12 C23_12 C1_11 108.0(2) . . ? C26_12 C23_12 C1_11 109.4(2) . . ? C24_12 C23_12 C1_11 111.0(2) . . ? C23_12 C24_12 H24A_12 109.5 . . ? C23_12 C24_12 H24B_12 109.5 . . ? H24A_12 C24_12 H24B_12 109.5 . . ? C23_12 C24_12 H24C_12 109.5 . . ? H24A_12 C24_12 H24C_12 109.5 . . ? H24B_12 C24_12 H24C_12 109.5 . . ? C23_12 C25_12 H25A_12 109.5 . . ? C23_12 C25_12 H25B_12 109.5 . . ? H25A_12 C25_12 H25B_12 109.5 . . ? C23_12 C25_12 H25C_12 109.5 . . ? H25A_12 C25_12 H25C_12 109.5 . . ? H25B_12 C25_12 H25C_12 109.5 . . ? C23_12 C26_12 H26A_12 109.5 . . ? C23_12 C26_12 H26B_12 109.5 . . ? H26A_12 C26_12 H26B_12 109.5 . . ? C23_12 C26_12 H26C_12 109.5 . . ? H26A_12 C26_12 H26C_12 109.5 . . ? H26B_12 C26_12 H26C_12 109.5 . . ? C26_120 C23_120 C24_120 109.5 . . ? C26_120 C23_120 C25_120 109.5 . . ? C24_120 C23_120 C25_120 109.5 . . ? C26_120 C23_120 C1_11 105.9(3) . . ? C24_120 C23_120 C1_11 111.9(3) . . ? C25_120 C23_120 C1_11 110.5(3) . . ? C23_120 C24_120 H24A_120 109.5 . . ? C23_120 C24_120 H24B_120 109.5 . . ? H24A_120 C24_120 H24B_120 109.5 . . ? C23_120 C24_120 H24C_120 109.5 . . ? H24A_120 C24_120 H24C_120 109.5 . . ? H24B_120 C24_120 H24C_120 109.5 . . ? C23_120 C25_120 H25A_120 109.5 . . ? C23_120 C25_120 H25B_120 109.5 . . ? H25A_120 C25_120 H25B_120 109.5 . . ? C23_120 C25_120 H25C_120 109.5 . . ? H25A_120 C25_120 H25C_120 109.5 . . ? H25B_120 C25_120 H25C_120 109.5 . . ? C23_120 C26_120 H26A_120 109.5 . . ? C23_120 C26_120 H26B_120 109.5 . . ? H26A_120 C26_120 H26B_120 109.5 . . ? C23_120 C26_120 H26C_120 109.5 . . ? H26A_120 C26_120 H26C_120 109.5 . . ? H26B_120 C26_120 H26C_120 109.5 . . ? C28_13 C27_13 C29_13 107.79(19) . . ? C28_13 C27_13 C30_13 109.2(2) . . ? C29_13 C27_13 C30_13 109.34(19) . . ? C28_13 C27_13 C8_11 111.93(18) . . ? C29_13 C27_13 C8_11 110.09(17) . . ? C30_13 C27_13 C8_11 108.48(17) . . ? C27_13 C28_13 H28A_13 109.5 . . ? C27_13 C28_13 H28B_13 109.5 . . ? H28A_13 C28_13 H28B_13 109.5 . . ? C27_13 C28_13 H28C_13 109.5 . . ? H28A_13 C28_13 H28C_13 109.5 . . ? H28B_13 C28_13 H28C_13 109.5 . . ? C27_13 C29_13 H29A_13 109.5 . . ? C27_13 C29_13 H29B_13 109.5 . . ? H29A_13 C29_13 H29B_13 109.5 . . ? C27_13 C29_13 H29C_13 109.5 . . ? H29A_13 C29_13 H29C_13 109.5 . . ? H29B_13 C29_13 H29C_13 109.5 . . ? C27_13 C30_13 H30A_13 109.5 . . ? C27_13 C30_13 H30B_13 109.5 . . ? H30A_13 C30_13 H30B_13 109.5 . . ? C27_13 C30_13 H30C_13 109.5 . . ? H30A_13 C30_13 H30C_13 109.5 . . ? H30B_13 C30_13 H30C_13 109.5 . . ? C32_13 C31_13 C14_11 112.03(16) . . ? C32_13 C31_13 C34_13 109.20(17) . . ? C14_11 C31_13 C34_13 110.17(16) . . ? C32_13 C31_13 C33_13 108.23(17) . . ? C14_11 C31_13 C33_13 108.16(16) . . ? C34_13 C31_13 C33_13 108.98(17) . . ? C31_13 C32_13 H32A_13 109.5 . . ? C31_13 C32_13 H32B_13 109.5 . . ? H32A_13 C32_13 H32B_13 109.5 . . ? C31_13 C32_13 H32C_13 109.5 . . ? H32A_13 C32_13 H32C_13 109.5 . . ? H32B_13 C32_13 H32C_13 109.5 . . ? C31_13 C33_13 H33A_13 109.5 . . ? C31_13 C33_13 H33B_13 109.5 . . ? H33A_13 C33_13 H33B_13 109.5 . . ? C31_13 C33_13 H33C_13 109.5 . . ? H33A_13 C33_13 H33C_13 109.5 . . ? H33B_13 C33_13 H33C_13 109.5 . . ? C31_13 C34_13 H34A_13 109.5 . . ? C31_13 C34_13 H34B_13 109.5 . . ? H34A_13 C34_13 H34B_13 109.5 . . ? C31_13 C34_13 H34C_13 109.5 . . ? H34A_13 C34_13 H34C_13 109.5 . . ? H34B_13 C34_13 H34C_13 109.5 . . ? Cl2_3 C1_3 Cl3_3 112.47(16) . . ? Cl2_3 C1_3 H1A_3 109.1 . . ? Cl3_3 C1_3 H1A_3 109.1 . . ? Cl2_3 C1_3 H1B_3 109.1 . . ? Cl3_3 C1_3 H1B_3 109.1 . . ? H1A_3 C1_3 H1B_3 107.8 . . ? Cl3_4 C1_4 Cl2_4 111.96(18) . . ? Cl3_4 C1_4 H1A_4 109.2 . . ? Cl2_4 C1_4 H1A_4 109.2 . . ? Cl3_4 C1_4 H1B_4 109.2 . . ? Cl2_4 C1_4 H1B_4 109.2 . . ? H1A_4 C1_4 H1B_4 107.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1_1 C2_1 1.388(3) . ? C1_1 C20_1 1.407(3) . ? C1_1 C23_1 1.534(3) . ? C2_1 C3_1 1.404(3) . ? C2_1 H2_1 0.9500 . ? C3_1 C21_1 1.419(3) . ? C3_1 C4_1 1.434(3) . ? C4_1 C5_1 1.353(3) . ? C4_1 H4_1 0.9500 . ? C5_1 C6_1 1.434(3) . ? C5_1 H5_1 0.9500 . ? C6_1 C7_1 1.403(3) . ? C6_1 C22_1 1.419(3) . ? C7_1 C8_1 1.383(3) . ? C7_1 H7_1 0.9500 . ? C8_1 C9_1 1.410(3) . ? C8_1 C27_20 1.548(2) . ? C8_1 C27_2 1.548(2) . ? C9_1 C10_1 1.398(3) . ? C9_1 H9_1 0.9500 . ? C10_1 C22_1 1.418(3) . ? C10_1 C11_1 1.462(3) . ? C11_1 C18_1 1.392(3) . ? C11_1 C12_1 1.460(3) . ? C12_1 C13_1 1.403(3) . ? C12_1 C17_1 1.413(3) . ? C13_1 C14_1 1.398(3) . ? C13_1 H13_1 0.9500 . ? C14_1 C15_1 1.394(3) . ? C14_1 C31 1.537(3) . ? C15_1 C16_1 1.407(3) . ? C15_1 H15_1 0.9500 . ? C16_1 C17_1 1.419(3) . ? C16_1 C18_1 1.459(3) 2_657 ? C17_1 C17_1 1.429(4) 2_657 ? C18_1 C19_1 1.464(3) . ? C19_1 C20_1 1.398(3) . ? C19_1 C21_1 1.419(3) . ? C20_1 H20_1 0.9500 . ? C21_1 C22_1 1.424(3) . ? C23_1 C25_1 1.529(4) . ? C23_1 C24_1 1.531(3) . ? C23_1 C26_1 1.539(4) . ? C24_1 H24A_1 0.9800 . ? C24_1 H24B_1 0.9800 . ? C24_1 H24C_1 0.9800 . ? C25_1 H25A_1 0.9800 . ? C25_1 H25B_1 0.9800 . ? C25_1 H25C_1 0.9800 . ? C26_1 H26A_1 0.9800 . ? C26_1 H26B_1 0.9800 . ? C26_1 H26C_1 0.9800 . ? C27_2 C28_2 1.5300 . ? C27_2 C29_2 1.5300 . ? C27_2 C30_2 1.5300 . ? C28_2 H28A_2 0.9800 . ? C28_2 H28B_2 0.9800 . ? C28_2 H28C_2 0.9800 . ? C29_2 H29A_2 0.9800 . ? C29_2 H29B_2 0.9800 . ? C29_2 H29C_2 0.9800 . ? C30_2 H30A_2 0.9800 . ? C30_2 H30B_2 0.9800 . ? C30_2 H30C_2 0.9800 . ? C27_20 C28_20 1.5300 . ? C27_20 C30_20 1.5300 . ? C27_20 C29_20 1.5300 . ? C28_20 H28A_20 0.9800 . ? C28_20 H28B_20 0.9800 . ? C28_20 H28C_20 0.9800 . ? C29_20 H29A_20 0.9800 . ? C29_20 H29B_20 0.9800 . ? C29_20 H29C_20 0.9800 . ? C30_20 H30A_20 0.9800 . ? C30_20 H30B_20 0.9800 . ? C30_20 H30C_20 0.9800 . ? C31 C33 1.530(3) . ? C31 C32 1.533(3) . ? C31 C34 1.536(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C1_11 C2_11 1.388(3) . ? C1_11 C20_11 1.398(3) . ? C1_11 C23_120 1.547(3) . ? C1_11 C23_12 1.549(3) . ? C2_11 C3_11 1.402(3) . ? C2_11 H2_11 0.9500 . ? C3_11 C21_11 1.414(3) . ? C3_11 C4_11 1.438(3) . ? C4_11 C5_11 1.357(3) . ? C4_11 H4_11 0.9500 . ? C5_11 C6_11 1.437(3) . ? C5_11 H5_11 0.9500 . ? C6_11 C7_11 1.405(3) . ? C6_11 C22_11 1.415(3) . ? C7_11 C8_11 1.387(3) . ? C7_11 H7_11 0.9500 . ? C8_11 C9_11 1.406(3) . ? C8_11 C27_13 1.536(3) . ? C9_11 C10_11 1.399(3) . ? C9_11 H9_11 0.9500 . ? C10_11 C22_11 1.419(3) . ? C10_11 C11_11 1.464(3) . ? C11_11 C18_11 1.395(3) . ? C11_11 C12_11 1.459(3) . ? C12_11 C13_11 1.408(3) . ? C12_11 C17_11 1.419(3) . ? C13_11 C14_11 1.394(3) . ? C13_11 H13_11 0.9500 . ? C14_11 C15_11 1.398(3) . ? C14_11 C31_13 1.536(3) . ? C15_11 C16_11 1.402(3) . ? C15_11 H15_11 0.9500 . ? C16_11 C17_11 1.414(3) . ? C16_11 C18_11 1.456(3) 2_566 ? C17_11 C17_11 1.431(4) 2_566 ? C18_11 C19_11 1.459(3) . ? C19_11 C20_11 1.405(3) . ? C19_11 C21_11 1.416(3) . ? C20_11 H20_11 0.9500 . ? C21_11 C22_11 1.428(3) . ? C23_12 C25_12 1.5299 . ? C23_12 C26_12 1.5300 . ? C23_12 C24_12 1.5300 . ? C24_12 H24A_12 0.9800 . ? C24_12 H24B_12 0.9800 . ? C24_12 H24C_12 0.9800 . ? C25_12 H25A_12 0.9800 . ? C25_12 H25B_12 0.9800 . ? C25_12 H25C_12 0.9800 . ? C26_12 H26A_12 0.9800 . ? C26_12 H26B_12 0.9800 . ? C26_12 H26C_12 0.9800 . ? C23_120 C26_120 1.5300 . ? C23_120 C24_120 1.5300 . ? C23_120 C25_120 1.5300 . ? C24_120 H24A_120 0.9800 . ? C24_120 H24B_120 0.9800 . ? C24_120 H24C_120 0.9800 . ? C25_120 H25A_120 0.9800 . ? C25_120 H25B_120 0.9800 . ? C25_120 H25C_120 0.9800 . ? C26_120 H26A_120 0.9800 . ? C26_120 H26B_120 0.9800 . ? C26_120 H26C_120 0.9800 . ? C27_13 C28_13 1.531(3) . ? C27_13 C29_13 1.533(3) . ? C27_13 C30_13 1.535(3) . ? C28_13 H28A_13 0.9800 . ? C28_13 H28B_13 0.9800 . ? C28_13 H28C_13 0.9800 . ? C29_13 H29A_13 0.9800 . ? C29_13 H29B_13 0.9800 . ? C29_13 H29C_13 0.9800 . ? C30_13 H30A_13 0.9800 . ? C30_13 H30B_13 0.9800 . ? C30_13 H30C_13 0.9800 . ? C31_13 C32_13 1.530(3) . ? C31_13 C34_13 1.537(3) . ? C31_13 C33_13 1.539(3) . ? C32_13 H32A_13 0.9800 . ? C32_13 H32B_13 0.9800 . ? C32_13 H32C_13 0.9800 . ? C33_13 H33A_13 0.9800 . ? C33_13 H33B_13 0.9800 . ? C33_13 H33C_13 0.9800 . ? C34_13 H34A_13 0.9800 . ? C34_13 H34B_13 0.9800 . ? C34_13 H34C_13 0.9800 . ? C1_3 Cl2_3 1.740(3) . ? C1_3 Cl3_3 1.746(3) . ? C1_3 H1A_3 0.9900 . ? C1_3 H1B_3 0.9900 . ? C1_4 Cl3_4 1.746(4) . ? C1_4 Cl2_4 1.755(3) . ? C1_4 H1A_4 0.9900 . ? C1_4 H1B_4 0.9900 . ?